# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2024

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

data_hxq_220503_1_197k_auto
_database_code_depnum_ccdc_archive 'CCDC 2195159'
loop_
_audit_author_name
_audit_author_address
'Zhong-Xia Wang'
;Nanchang University
China
;
_audit_update_record             
;
2022-08-05 deposited with the CCDC.	2023-12-03 downloaded from the CCDC.
;
_audit_creation_date             2022-05-16
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br3 Pb, C5 H12 N'
_chemical_formula_sum            'C6 H12 Br3 N0.25 Pb'
_chemical_formula_weight         534.58
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C N H Pb  Br'
_chemical_oxdiff_usercomment     \
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'
Pb Pb -3.3944 10.1111 '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'

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

_cell_length_a                   9.6329(3)
_cell_length_b                   7.9359(2)
_cell_length_c                   14.9282(5)
_cell_angle_alpha                90
_cell_angle_beta                 102.867(3)
_cell_angle_gamma                90
_cell_volume                     1112.54(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5725
_cell_measurement_temperature    197.0(2)
_cell_measurement_theta_max      30.7870
_cell_measurement_theta_min      2.1140
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    25.880
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.05279
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.108a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.192
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       strip
_exptl_crystal_F_000             947
_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  0.0421
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.802
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8699
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.802
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.701
_diffrn_reflns_theta_min         2.304
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      197.0(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.802
_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  24.00   0.50    1.00    --    5.04  49.00  83.00   64
  2  ω     28.00  77.00   0.50    1.00    --    5.04  49.00  83.00   98
  3  ω    -18.00   8.00   0.50    1.00    --    5.04 -99.00  90.00   52
  4  ω    -58.00  18.00   0.50    1.00    --    5.04 -49.00 -63.00  152
  5  ω    -18.00   9.00   0.50    1.00    --   -5.19 -99.00 -60.00   54
  6  ω    -16.00  15.00   0.50    1.00    --   -5.19 -99.00-180.00   62
;
_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      0.0562315000
_diffrn_orient_matrix_UB_12      -0.0527553000
_diffrn_orient_matrix_UB_13      0.0228892000
_diffrn_orient_matrix_UB_21      0.0236648000
_diffrn_orient_matrix_UB_22      -0.0092358000
_diffrn_orient_matrix_UB_23      -0.0414456000
_diffrn_orient_matrix_UB_31      0.0445257000
_diffrn_orient_matrix_UB_32      0.0715740000
_diffrn_orient_matrix_UB_33      0.0115375000
_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                2413
_reflns_number_total             2769
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_refine_diff_density_max         5.097
_refine_diff_density_min         -2.890
_refine_diff_density_rms         0.422
_refine_ls_extinction_coef       0.0053(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     92
_refine_ls_number_reflns         2769
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0446
_refine_ls_restrained_S_all      1.059
_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)+(0.1013P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1317
_refine_ls_wR_factor_ref         0.1374
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 N8(H8A,H8B), C5(H5A,H5B), C9(H9A,H9B), C6(H6A,H6B), C7(H7A,H7B), C10(H10A,H10B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.25439(3) 0.51354(4) 0.24477(2) 0.02122(17) Uani 1 1 d . . . . .
Br2 Br 0.30823(9) 0.31435(10) 0.40848(5) 0.0250(2) Uani 1 1 d . . . . .
Br3 Br 0.06024(9) 0.72336(10) 0.32215(6) 0.0250(2) Uani 1 1 d . . . . .
Br4 Br 0.47349(9) 0.75031(9) 0.33944(6) 0.0265(2) Uani 1 1 d . . . . .
N8 N 0.3153(8) 0.6980(10) 0.5323(5) 0.0311(16) Uani 1 1 d . . . . .
H8A H 0.255383 0.686787 0.476164 0.037 Uiso 1 1 calc R U . . .
H8B H 0.400862 0.653001 0.528983 0.037 Uiso 1 1 calc R U . . .
C5 C 0.1366(12) 0.8633(12) 0.6370(7) 0.040(2) Uani 1 1 d . . . . .
H5A H 0.203161 0.874336 0.697697 0.049 Uiso 1 1 calc R U . . .
H5B H 0.044077 0.912532 0.641782 0.049 Uiso 1 1 calc R U . . .
C9 C 0.2557(11) 0.6019(11) 0.6025(6) 0.034(2) Uani 1 1 d . . . . .
H9A H 0.324633 0.604265 0.662553 0.041 Uiso 1 1 calc R U . . .
H9B H 0.239819 0.482845 0.583079 0.041 Uiso 1 1 calc R U . . .
C6 C 0.1946(11) 0.9586(11) 0.5661(7) 0.034(2) Uani 1 1 d . . . . .
H6A H 0.209265 1.078116 0.584816 0.041 Uiso 1 1 calc R U . . .
H6B H 0.124979 0.954548 0.506340 0.041 Uiso 1 1 calc R U . . .
C7 C 0.3344(9) 0.8827(11) 0.5559(6) 0.0316(19) Uani 1 1 d . . . . .
H7A H 0.368690 0.942406 0.506738 0.038 Uiso 1 1 calc R U . . .
H7B H 0.406628 0.896316 0.613998 0.038 Uiso 1 1 calc R U . . .
C10 C 0.1168(13) 0.6799(13) 0.6120(8) 0.046(3) Uani 1 1 d . . . . .
H10A H 0.045499 0.668434 0.553306 0.055 Uiso 1 1 calc R U . . .
H10B H 0.080485 0.619578 0.660141 0.055 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 Br2 2.8593(8) . ?
Pb1 Br3 2.9270(9) . ?
Pb1 Br3 3.2069(9) 2_545 ?
Pb1 Br4 3.0876(9) 2_545 ?
Pb1 Br4 2.9418(8) . ?
N8 H8A 0.9100 . ?
N8 H8B 0.9100 . ?
N8 C9 1.509(12) . ?
N8 C7 1.509(11) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.506(13) . ?
C5 C10 1.504(15) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C10 1.509(14) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 C7 1.514(13) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?

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
Br2 Pb1 Br3 89.28(2) . . ?
Br2 Pb1 Br3 82.05(2) . 2_545 ?
Br2 Pb1 Br4 87.20(2) . 2_545 ?
Br2 Pb1 Br4 88.19(2) . . ?
Br3 Pb1 Br3 168.67(3) . 2_545 ?
Br3 Pb1 Br4 84.27(3) . . ?
Br3 Pb1 Br4 94.97(2) . 2_545 ?
Br4 Pb1 Br3 77.41(2) 2_545 2_545 ?
Br4 Pb1 Br3 102.63(2) . 2_545 ?
Br4 Pb1 Br4 175.333(17) . 2_545 ?
Pb1 Br3 Pb1 80.59(2) . 2 ?
Pb1 Br4 Pb1 82.39(2) . 2 ?
H8A N8 H8B 107.9 . . ?
C9 N8 H8A 109.2 . . ?
C9 N8 H8B 109.2 . . ?
C9 N8 C7 112.0(7) . . ?
C7 N8 H8A 109.2 . . ?
C7 N8 H8B 109.2 . . ?
H5A C5 H5B 108.0 . . ?
C6 C5 H5A 109.4 . . ?
C6 C5 H5B 109.4 . . ?
C10 C5 H5A 109.4 . . ?
C10 C5 H5B 109.4 . . ?
C10 C5 C6 110.9(8) . . ?
N8 C9 H9A 109.7 . . ?
N8 C9 H9B 109.7 . . ?
N8 C9 C10 109.9(7) . . ?
H9A C9 H9B 108.2 . . ?
C10 C9 H9A 109.7 . . ?
C10 C9 H9B 109.7 . . ?
C5 C6 H6A 109.6 . . ?
C5 C6 H6B 109.6 . . ?
C5 C6 C7 110.4(8) . . ?
H6A C6 H6B 108.1 . . ?
C7 C6 H6A 109.6 . . ?
C7 C6 H6B 109.6 . . ?
N8 C7 C6 110.2(7) . . ?
N8 C7 H7A 109.6 . . ?
N8 C7 H7B 109.6 . . ?
C6 C7 H7A 109.6 . . ?
C6 C7 H7B 109.6 . . ?
H7A C7 H7B 108.1 . . ?
C5 C10 C9 110.8(9) . . ?
C5 C10 H10A 109.5 . . ?
C5 C10 H10B 109.5 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 108.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N8 C9 C10 C5 -56.6(11) . . . . ?
C5 C6 C7 N8 56.2(10) . . . . ?
C9 N8 C7 C6 -56.3(10) . . . . ?
C6 C5 C10 C9 58.1(12) . . . . ?
C7 N8 C9 C10 56.3(10) . . . . ?
C10 C5 C6 C7 -57.7(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 8.739
_oxdiff_exptl_absorpt_empirical_full_min 0.390
####################################################################### 
# 
# 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_PDPbBr3_423K
_database_code_depnum_ccdc_archive 'CCDC 2195161'
loop_
_audit_author_name
_audit_author_address
'Zhong-Xia Wang'
;Nanchang University
China
;
_audit_update_record             
;
2022-08-05 deposited with the CCDC.	2023-12-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 N, Br3 Pb, 0.25(C4)'
_chemical_formula_sum            'C5 Br3 N Pb'
_chemical_formula_weight         520.96

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'
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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_H-M_alt        'C m c m'
_space_group_name_Hall           '-C 2c 2'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, 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'
'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, y, z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z-1/2'
'-x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   8.2943(6)
_cell_length_b                   18.2287(15)
_cell_length_c                   7.8044(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1179.98(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    423(2)
_cell_measurement_reflns_used    1423
_cell_measurement_theta_min      2.2080
_cell_measurement_theta_max      28.8070

_exptl_crystal_description       strip
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_F_000             448
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    12.200
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      423(2)
_diffrn_radiation_wavelength     0.710
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            2957
_diffrn_reflns_av_unetI/netI     0.0547
_diffrn_reflns_av_R_equivalents  0.0782
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.232
_diffrn_reflns_theta_max         30.272
_diffrn_reflns_theta_full        25.214
_diffrn_measured_fraction_theta_max 0.858
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.858
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.858
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             856
_reflns_number_gt                588
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1216P)²+1.4125P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.024(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         856
_refine_ls_number_parameters     64
_refine_ls_number_restraints     103
_refine_ls_R_factor_all          0.0904
_refine_ls_R_factor_gt           0.0658
_refine_ls_wR_factor_ref         0.2058
_refine_ls_wR_factor_gt          0.1889
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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 0.0000 1.0000 0.5000 0.0692(6) Uani 0.5 4 d S TU P . .
Br1 Br 0.0000 0.87172(16) 0.7500 0.0934(10) Uani 0.5 4 d S TU P . .
Br2 Br 0.2487(3) 1.05793(14) 0.7500 0.1060(9) Uani 0.5 2 d S TU P . .
C1 C 0.544(6) 0.1188(19) 0.109(5) 0.104(8) Uani 0.125 1 d D U P . .
C2 C 0.552(8) 0.195(2) 0.051(4) 0.100(8) Uani 0.125 1 d D U P . .
C3 C 0.575(7) 0.2523(17) 0.180(5) 0.101(8) Uani 0.125 1 d D U P . .
C5 C 0.468(9) 0.163(2) 0.398(4) 0.107(8) Uani 0.125 1 d D U P . .
C4 C 0.5000 0.2394(17) 0.347(5) 0.104(8) Uani 0.25 2 d DS TU P . .
N1 N 0.444(4) 0.1104(15) 0.2500 0.109(8) Uani 0.25 2 d DS TU P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br2 3.0295(16) 9_576 ?
Pb1 Br2 3.0295(16) 11 ?
Pb1 Br2 3.0295(16) 3_576 ?
Pb1 Br2 3.0295(16) . ?
Pb1 Br1 3.045(2) 9_576 ?
Pb1 Br1 3.045(2) . ?
Br1 Pb1 3.045(2) 2_575 ?
Br2 Pb1 3.0295(16) 2_575 ?
C1 C1 0.73(11) 11_655 ?
C1 C5 0.81(4) 4_655 ?
C1 C5 1.03(6) 10_556 ?
C1 N1 1.11(4) 11_655 ?
C1 N1 1.39(3) . ?
C1 C2 1.46(3) . ?
C1 C2 1.66(5) 11_655 ?
C2 C5 0.72(5) 4_655 ?
C2 C2 0.86(13) 11_655 ?
C2 C5 0.99(6) 10_556 ?
C2 C4 1.22(7) 10_556 ?
C2 C3 1.47(3) . ?
C2 C1 1.66(5) 11_655 ?
C2 C3 1.80(5) 11_655 ?
C3 C4 0.70(5) 10_556 ?
C3 C3 1.09(8) 10_556 ?
C3 C3 1.25(11) 11_655 ?
C3 C4 1.46(2) . ?
C3 C3 1.66(10) 4_655 ?
C3 C5 1.77(6) 4_655 ?
C3 C2 1.80(5) 11_655 ?
C3 C5 1.95(5) 10_556 ?
C5 C5 0.54(14) 11_655 ?
C5 C2 0.72(5) 4_655 ?
C5 C1 0.81(4) 4_655 ?
C5 C2 0.99(6) 10_556 ?
C5 C1 1.03(6) 10_556 ?
C5 C4 1.47(3) . ?
C5 N1 1.51(3) . ?
C5 N1 1.67(4) 11_655 ?
C5 C3 1.77(6) 4_655 ?
C5 C3 1.95(5) 10_556 ?
C4 C3 0.70(5) 4_655 ?
C4 C3 0.70(5) 10_556 ?
C4 C2 1.22(7) 4_655 ?
C4 C2 1.22(7) 10_556 ?
C4 C3 1.46(2) 11_655 ?
C4 C5 1.47(3) 11_655 ?
C4 C4 1.51(8) 10_556 ?
N1 N1 0.93(7) 11_655 ?
N1 C1 1.11(4) 4_655 ?
N1 C1 1.11(4) 11_655 ?
N1 C1 1.39(3) 10_556 ?
N1 C5 1.51(3) 10_556 ?
N1 C5 1.67(4) 11_655 ?
N1 C5 1.67(4) 4_655 ?

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
Br2 Pb1 Br2 94.16(7) 9_576 11 ?
Br2 Pb1 Br2 85.84(7) 9_576 3_576 ?
Br2 Pb1 Br2 180.0 11 3_576 ?
Br2 Pb1 Br2 180.00(6) 9_576 . ?
Br2 Pb1 Br2 85.84(7) 11 . ?
Br2 Pb1 Br2 94.16(7) 3_576 . ?
Br2 Pb1 Br1 81.66(5) 9_576 9_576 ?
Br2 Pb1 Br1 98.34(5) 11 9_576 ?
Br2 Pb1 Br1 81.66(5) 3_576 9_576 ?
Br2 Pb1 Br1 98.34(5) . 9_576 ?
Br2 Pb1 Br1 98.34(5) 9_576 . ?
Br2 Pb1 Br1 81.66(5) 11 . ?
Br2 Pb1 Br1 98.34(5) 3_576 . ?
Br2 Pb1 Br1 81.66(5) . . ?
Br1 Pb1 Br1 180.0 9_576 . ?
Pb1 Br1 Pb1 79.68(7) 2_575 . ?
Pb1 Br2 Pb1 80.19(5) . 2_575 ?
C1 C1 C5 83(7) 11_655 4_655 ?
C1 C1 C5 52(3) 11_655 10_556 ?
C5 C1 C5 31(9) 4_655 10_556 ?
C1 C1 N1 95(4) 11_655 11_655 ?
C5 C1 N1 102(4) 4_655 11_655 ?
C5 C1 N1 102(4) 10_556 11_655 ?
C1 C1 N1 53(3) 11_655 . ?
C5 C1 N1 95(5) 4_655 . ?
C5 C1 N1 76(3) 10_556 . ?
N1 C1 N1 42(4) 11_655 . ?
C1 C1 C2 93(3) 11_655 . ?
C5 C1 C2 17(4) 4_655 . ?
C5 C1 C2 43(3) 10_556 . ?
N1 C1 C2 116(2) 11_655 . ?
N1 C1 C2 112(3) . . ?
C1 C1 C2 61(3) 11_655 11_655 ?
C5 C1 C2 26(6) 4_655 11_655 ?
C5 C1 C2 15(4) 10_556 11_655 ?
N1 C1 C2 115(3) 11_655 11_655 ?
N1 C1 C2 91(3) . 11_655 ?
C2 C1 C2 31(5) . 11_655 ?
C5 C2 C2 77(9) 4_655 11_655 ?
C5 C2 C5 32(10) 4_655 10_556 ?
C2 C2 C5 45(4) 11_655 10_556 ?
C5 C2 C4 95(6) 4_655 10_556 ?
C2 C2 C4 69(3) 11_655 10_556 ?
C5 C2 C4 83(4) 10_556 10_556 ?
C5 C2 C1 19(4) 4_655 . ?
C2 C2 C1 87(3) 11_655 . ?
C5 C2 C1 45(4) 10_556 . ?
C4 C2 C1 115(3) 10_556 . ?
C5 C2 C3 103(5) 4_655 . ?
C2 C2 C3 98(3) 11_655 . ?
C5 C2 C3 104(4) 10_556 . ?
C4 C2 C3 28(2) 10_556 . ?
C1 C2 C3 118(2) . . ?
C5 C2 C1 22(7) 4_655 11_655 ?
C2 C2 C1 61(3) 11_655 11_655 ?
C5 C2 C1 21(4) 10_556 11_655 ?
C4 C2 C1 102(3) 10_556 11_655 ?
C1 C2 C1 26(4) . 11_655 ?
C3 C2 C1 118(2) . 11_655 ?
C5 C2 C3 91(6) 4_655 11_655 ?
C2 C2 C3 54(2) 11_655 11_655 ?
C5 C2 C3 73(4) 10_556 11_655 ?
C4 C2 C3 15(2) 10_556 11_655 ?
C1 C2 C3 111(3) . 11_655 ?
C3 C2 C3 44(4) . 11_655 ?
C1 C2 C3 93(3) 11_655 11_655 ?
C4 C3 C3 107(6) 10_556 10_556 ?
C4 C3 C3 27(6) 10_556 11_655 ?
C3 C3 C3 90.001(11) 10_556 11_655 ?
C4 C3 C4 80(7) 10_556 . ?
C3 C3 C4 27(2) 10_556 . ?
C3 C3 C4 65(2) 11_655 . ?
C4 C3 C2 56(5) 10_556 . ?
C3 C3 C2 133.2(15) 10_556 . ?
C3 C3 C2 82(3) 11_655 . ?
C4 C3 C2 116.0(18) . . ?
C4 C3 C3 62(7) 10_556 4_655 ?
C3 C3 C3 49(4) 10_556 4_655 ?
C3 C3 C3 41(4) 11_655 4_655 ?
C4 C3 C3 25(2) . 4_655 ?
C2 C3 C3 111(4) . 4_655 ?
C4 C3 C5 54(4) 10_556 4_655 ?
C3 C3 C5 110.0(18) 10_556 4_655 ?
C3 C3 C5 78(3) 11_655 4_655 ?
C4 C3 C5 94(2) . 4_655 ?
C2 C3 C5 23.3(18) . 4_655 ?
C3 C3 C5 94(3) 4_655 4_655 ?
C4 C3 C2 27(6) 10_556 11_655 ?
C3 C3 C2 124.0(16) 10_556 11_655 ?
C3 C3 C2 54(2) 11_655 11_655 ?
C4 C3 C2 99(3) . 11_655 ?
C2 C3 C2 28(4) . 11_655 ?
C3 C3 C2 86(4) 4_655 11_655 ?
C5 C3 C2 32(2) 4_655 11_655 ?
C4 C3 C5 39(4) 10_556 10_556 ?
C3 C3 C5 108.1(16) 10_556 10_556 ?
C3 C3 C5 63(3) 11_655 10_556 ?
C4 C3 C5 87(2) . 10_556 ?
C2 C3 C5 30(2) . 10_556 ?
C3 C3 C5 82(3) 4_655 10_556 ?
C5 C3 C5 16(4) 4_655 10_556 ?
C2 C3 C5 21.6(17) 11_655 10_556 ?
C5 C5 C2 103(9) 11_655 4_655 ?
C5 C5 C1 97(7) 11_655 4_655 ?
C2 C5 C1 143(8) 4_655 4_655 ?
C5 C5 C2 45(4) 11_655 10_556 ?
C2 C5 C2 58(10) 4_655 10_556 ?
C1 C5 C2 133(10) 4_655 10_556 ?
C5 C5 C1 52(3) 11_655 10_556 ?
C2 C5 C1 143(10) 4_655 10_556 ?
C1 C5 C1 45(7) 4_655 10_556 ?
C2 C5 C1 92(6) 10_556 10_556 ?
C5 C5 C4 79(3) 11_655 . ?
C2 C5 C4 55(5) 4_655 . ?
C1 C5 C4 160(4) 4_655 . ?
C2 C5 C4 55(4) 10_556 . ?
C1 C5 C4 128(5) 10_556 . ?
C5 C5 N1 97(3) 11_655 . ?
C2 C5 N1 154(10) 4_655 . ?
C1 C5 N1 46(3) 4_655 . ?
C2 C5 N1 140(5) 10_556 . ?
C1 C5 N1 63(2) 10_556 . ?
C4 C5 N1 114.7(19) . . ?
C5 C5 N1 64(3) 11_655 11_655 ?
C2 C5 N1 160(7) 4_655 11_655 ?
C1 C5 N1 56(3) 4_655 11_655 ?
C2 C5 N1 108(6) 10_556 11_655 ?
C1 C5 N1 41(3) 10_556 11_655 ?
C4 C5 N1 106(2) . 11_655 ?
N1 C5 N1 34(3) . 11_655 ?
C5 C5 C3 102(3) 11_655 4_655 ?
C2 C5 C3 54(4) 4_655 4_655 ?
C1 C5 C3 150(8) 4_655 4_655 ?
C2 C5 C3 75(4) 10_556 4_655 ?
C1 C5 C3 146(5) 10_556 4_655 ?
C4 C5 C3 23(2) . 4_655 ?
N1 C5 C3 107(3) . 4_655 ?
N1 C5 C3 112(3) 11_655 4_655 ?
C5 C5 C3 63(3) 11_655 10_556 ?
C2 C5 C3 67(5) 4_655 10_556 ?
C1 C5 C3 149(6) 4_655 10_556 ?
C2 C5 C3 47(2) 10_556 10_556 ?
C1 C5 C3 111(5) 10_556 10_556 ?
C4 C5 C3 17.2(19) . 10_556 ?
N1 C5 C3 111(3) . 10_556 ?
N1 C5 C3 94(3) 11_655 10_556 ?
C3 C5 C3 39(4) 4_655 10_556 ?
C3 C4 C3 127(10) 4_655 10_556 ?
C3 C4 C2 96(6) 4_655 4_655 ?
C3 C4 C2 137(8) 10_556 4_655 ?
C3 C4 C2 137(8) 4_655 10_556 ?
C3 C4 C2 96(6) 10_556 10_556 ?
C2 C4 C2 41(6) 4_655 10_556 ?
C3 C4 C3 93(8) 4_655 . ?
C3 C4 C3 45(6) 10_556 . ?
C2 C4 C3 147(3) 4_655 . ?
C2 C4 C3 122(4) 10_556 . ?
C3 C4 C3 45(6) 4_655 11_655 ?
C3 C4 C3 93(8) 10_556 11_655 ?
C2 C4 C3 122(4) 4_655 11_655 ?
C2 C4 C3 147(3) 10_556 11_655 ?
C3 C4 C3 51(5) . 11_655 ?
C3 C4 C5 104(6) 4_655 . ?
C3 C4 C5 124(5) 10_556 . ?
C2 C4 C5 29(2) 4_655 . ?
C2 C4 C5 42(3) 10_556 . ?
C3 C4 C5 118.0(18) . . ?
C3 C4 C5 108(3) 11_655 . ?
C3 C4 C5 124(5) 4_655 11_655 ?
C3 C4 C5 104(6) 10_556 11_655 ?
C2 C4 C5 42(3) 4_655 11_655 ?
C2 C4 C5 29(2) 10_556 11_655 ?
C3 C4 C5 108(3) . 11_655 ?
C3 C4 C5 118.0(18) 11_655 11_655 ?
C5 C4 C5 21(6) . 11_655 ?
C3 C4 C4 73(6) 4_655 10_556 ?
C3 C4 C4 73(6) 10_556 10_556 ?
C2 C4 C4 131(3) 4_655 10_556 ?
C2 C4 C4 131(3) 10_556 10_556 ?
C3 C4 C4 27(2) . 10_556 ?
C3 C4 C4 27(2) 11_655 10_556 ?
C5 C4 C4 105.6(15) . 10_556 ?
C5 C4 C4 105.6(15) 11_655 10_556 ?
N1 N1 C1 85(4) 11_655 4_655 ?
N1 N1 C1 85(4) 11_655 11_655 ?
C1 N1 C1 161(5) 4_655 11_655 ?
N1 N1 C1 53(3) 11_655 10_556 ?
C1 N1 C1 32(5) 4_655 10_556 ?
C1 N1 C1 136(3) 11_655 10_556 ?
N1 N1 C1 53(3) 11_655 . ?
C1 N1 C1 136(3) 4_655 . ?
C1 N1 C1 32(5) 11_655 . ?
C1 N1 C1 105(5) 10_556 . ?
N1 N1 C5 83(3) 11_655 10_556 ?
C1 N1 C5 131(2) 4_655 10_556 ?
C1 N1 C5 32(2) 11_655 10_556 ?
C1 N1 C5 117(3) 10_556 10_556 ?
C1 N1 C5 41(3) . 10_556 ?
N1 N1 C5 83(3) 11_655 . ?
C1 N1 C5 32(2) 4_655 . ?
C1 N1 C5 131(2) 11_655 . ?
C1 N1 C5 41(3) 10_556 . ?
C1 N1 C5 117(3) . . ?
C5 N1 C5 99(3) 10_556 . ?
N1 N1 C5 64(3) 11_655 11_655 ?
C1 N1 C5 37(2) 4_655 11_655 ?
C1 N1 C5 124(4) 11_655 11_655 ?
C1 N1 C5 29.0(19) 10_556 11_655 ?
C1 N1 C5 103(3) . 11_655 ?
C5 N1 C5 96(2) 10_556 11_655 ?
C5 N1 C5 19(5) . 11_655 ?
N1 N1 C5 64(3) 11_655 4_655 ?
C1 N1 C5 124(4) 4_655 4_655 ?
C1 N1 C5 37(2) 11_655 4_655 ?
C1 N1 C5 103(3) 10_556 4_655 ?
C1 N1 C5 29.0(19) . 4_655 ?
C5 N1 C5 19(5) 10_556 4_655 ?
C5 N1 C5 96(2) . 4_655 ?
C5 N1 C5 87(4) 11_655 4_655 ?

_refine_diff_density_max         0.894
_refine_diff_density_min         -0.644
_refine_diff_density_rms         0.138



####################################################################### 
# 
# 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_hxq-211027-2-293k-3st_auto
_database_code_depnum_ccdc_archive 'CCDC 2195166'
loop_
_audit_author_name
_audit_author_address
'Zhong-Xia Wang'
;Nanchang University
China
;
_audit_update_record             
;
2022-08-05 deposited with the CCDC.	2023-12-03 downloaded from the CCDC.
;
_audit_creation_date             2022-01-18
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br8 Pb2, 4(C9)'
_chemical_formula_sum            'C36 Br8 Pb2'
_chemical_formula_weight         1486.02
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H  N F Pb Br'
_chemical_oxdiff_usercomment     \
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'
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           69
_space_group_name_H-M_alt        'F m m m'
_space_group_name_Hall           '-F 2 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y+1/2, -z+1/2'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'-x+1/2, y, -z+1/2'
'x+1/2, -y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-x, -y+1/2, -z+1/2'
'x, y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'
'-x, y+1/2, z+1/2'
'-x+1/2, -y, -z+1/2'
'x+1/2, y, -z+1/2'
'x+1/2, -y, z+1/2'
'-x+1/2, y, z+1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'

_cell_length_a                   8.6355(9)
_cell_length_b                   24.748(2)
_cell_length_c                   8.8106(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1882.9(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1309
_cell_measurement_temperature    293.1(4)
_cell_measurement_theta_max      27.8330
_cell_measurement_theta_min      3.2930
_shelx_estimated_absorpt_T_max   0.722
_shelx_estimated_absorpt_T_min   0.542
_exptl_absorpt_coefficient_mu    17.442
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.12171
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.108a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic light colourless'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.621
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.831
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2715
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.831
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.943
_diffrn_reflns_theta_min         3.293
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293.1(4)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.831
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -66.00  18.00   0.50    2.00    --    5.13 -37.00   0.00  168
  2  ω    -11.00  14.00   0.50    2.00    --    5.13-101.00  23.00   50
  3  ω    -18.00  23.00   0.50    2.00    --   -5.29 -99.00-150.00   82
  4  ω    -38.00 -11.00   0.50    2.00    --   -5.29 101.00 127.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0409171000
_diffrn_orient_matrix_UB_12      0.0238595000
_diffrn_orient_matrix_UB_13      -0.0196224000
_diffrn_orient_matrix_UB_21      -0.0316089000
_diffrn_orient_matrix_UB_22      -0.0011597000
_diffrn_orient_matrix_UB_23      -0.0742059000
_diffrn_orient_matrix_UB_31      -0.0638992000
_diffrn_orient_matrix_UB_32      0.0158095000
_diffrn_orient_matrix_UB_33      0.0240774000
_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                500
_reflns_number_total             709
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         2.925
_refine_diff_density_min         -1.332
_refine_diff_density_rms         0.270
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     40
_refine_ls_number_reflns         709
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0927
_refine_ls_R_factor_gt           0.0669
_refine_ls_restrained_S_all      1.003
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1414P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1862
_refine_ls_wR_factor_ref         0.1978
_refine_special_details          ?
_olex2_refinement_description    
;
1. Uiso/Uaniso restraints and constraints
C2 \\sim C3 \\sim C1 \\sim C6: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.01 within 2A
Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
2. Others
 Fixed Sof: C3(0.5)
;
_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 1.000000 0.500000 1.000000 0.06348(10) Uani 1 8 d S T P . .
Br02 Br 1.250000 0.500000 1.250000 0.0889(3) Uani 1 4 d S T P . .
Br03 Br 1.000000 0.61858(5) 1.000000 0.1488(7) Uani 1 4 d S T P . .
C3 C 0.581(3) 0.6175(8) 0.916(3) 0.2123(13) Uani 0.5 1 d . U P A 1
C1 C 0.500000 0.5985(10) 1.000000 0.2074(17) Uani 1 4 d S TU P . .
C2 C 0.500000 0.6825(7) 0.8111(19) 0.2216(13) Uani 1 2 d S TU P . .
C6 C 0.4215(10) 0.7001(4) 0.9085(11) 0.227(2) Uani 1 1 d . 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 Br02 3.0842(2) . ?
Pb01 Br02 3.0842(2) 10_764 ?
Pb01 Br02 3.0842(2) 2_765 ?
Pb01 Br02 3.0842(2) 9_454 ?
Pb01 Br03 2.9346(13) 17_767 ?
Pb01 Br03 2.9345(13) . ?
C3 C3 1.39(6) 20_655 ?
C3 C3 1.47(6) 18_557 ?
C3 C1 1.12(3) . ?
C3 C2 1.98(3) . ?
C2 C6 1.177(17) . ?
C2 C6 1.177(17) 20_655 ?
C6 C6 1.356(18) 20_655 ?
C6 C6 1.61(2) 18_557 ?

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 180.0 . 9_454 ?
Br02 Pb01 Br02 88.850(8) 9_454 10_764 ?
Br02 Pb01 Br02 91.150(8) . 10_764 ?
Br02 Pb01 Br02 180.0 2_765 10_764 ?
Br02 Pb01 Br02 91.150(8) 9_454 2_765 ?
Br02 Pb01 Br02 88.850(8) . 2_765 ?
Br03 Pb01 Br02 90.0 17_767 . ?
Br03 Pb01 Br02 90.0 17_767 9_454 ?
Br03 Pb01 Br02 90.0 . 2_765 ?
Br03 Pb01 Br02 90.0 . 9_454 ?
Br03 Pb01 Br02 90.0 . . ?
Br03 Pb01 Br02 90.0 . 10_764 ?
Br03 Pb01 Br02 90.0 17_767 10_764 ?
Br03 Pb01 Br02 90.0 17_767 2_765 ?
Br03 Pb01 Br03 180.0 . 17_767 ?
Pb01 Br02 Pb01 180.0 9 . ?
C3 C3 C3 90.001(15) 20_655 18_557 ?
C3 C3 C2 69.4(8) 20_655 . ?
C3 C3 C2 117.9(9) 18_557 . ?
C1 C3 C3 48.8(15) . 18_557 ?
C1 C3 C3 51.3(15) . 20_655 ?
C1 C3 C2 115(2) . . ?
C3 C1 C3 130(3) 18_557 20_655 ?
C3 C1 C3 130(3) . 3_657 ?
C3 C1 C3 77(3) . 20_655 ?
C3 C1 C3 82(3) 20_655 3_657 ?
C3 C1 C3 82(3) . 18_557 ?
C3 C1 C3 77(3) 18_557 3_657 ?
C3 C2 C3 41.1(16) 20_655 . ?
C6 C2 C3 99.3(14) . . ?
C6 C2 C3 76.0(12) . 20_655 ?
C6 C2 C3 99.3(14) 20_655 20_655 ?
C6 C2 C3 76.0(12) 20_655 . ?
C6 C2 C6 70.3(13) . 20_655 ?
C2 C6 C6 136.8(8) . 18_557 ?
C2 C6 C6 54.8(7) . 20_655 ?
C6 C6 C6 90.001(6) 20_655 18_557 ?

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 C3 C1 C3 -134(3) 20_655 . . 18_557 ?
C3 C3 C1 C3 66.1(18) 18_557 . . 3_657 ?
C3 C3 C1 C3 134(3) 18_557 . . 20_655 ?
C3 C3 C1 C3 -68.3(17) 20_655 . . 3_657 ?
C3 C2 C6 C6 64.0(12) 20_655 . . 18_557 ?
C3 C2 C6 C6 105.5(11) 20_655 . . 20_655 ?
C3 C2 C6 C6 71.4(10) . . . 20_655 ?
C3 C2 C6 C6 29.9(15) . . . 18_557 ?
C2 C3 C1 C3 -105.8(19) . . . 18_557 ?
C2 C3 C1 C3 -39.7(11) . . . 3_657 ?
C2 C3 C1 C3 29(3) . . . 20_655 ?
C6 C2 C6 C6 -41.5(16) 20_655 . . 18_557 ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.369
_oxdiff_exptl_absorpt_empirical_full_min 0.445

# start Validation Reply Form
_vrf_PLAT242_hxq-211027-2-293k-3st_auto 
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of       Pb01 Check 
RESPONSE: These alerts are generated because there is a large amount of disorder
;

# end Validation Reply Form


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

data_hxq-211027-2-420k-2st_auto
_database_code_depnum_ccdc_archive 'CCDC 2195167'
loop_
_audit_author_name
_audit_author_address
'Zhong-Xia Wang'
;Nanchang University
China
;
_audit_update_record             
;
2022-08-05 deposited with the CCDC.	2023-12-03 downloaded from the CCDC.
;
_audit_creation_date             2022-01-05
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br4 Pb, 4(C6.5)'
_chemical_formula_sum            'C26 Br4 Pb'
_chemical_formula_weight         839.09
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H  N F Pb Br'
_chemical_oxdiff_usercomment     \
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'
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      tetragonal
_space_group_IT_number           139
_space_group_name_H-M_alt        'I 4/m m m'
_space_group_name_Hall           '-I 4 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'-x, y, -z'
'x, -y, -z'
'y, x, -z'
'-y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'x, -y, z'
'-x, y, z'
'-y, -x, z'
'y, x, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'

_cell_length_a                   6.2229(5)
_cell_length_b                   6.2229(5)
_cell_length_c                   25.276(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     978.8(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    796
_cell_measurement_temperature    420.00(16)
_cell_measurement_theta_max      23.4460
_cell_measurement_theta_min      3.2120
_shelx_estimated_absorpt_T_max   0.730
_shelx_estimated_absorpt_T_min   0.553
_exptl_absorpt_coefficient_mu    16.796
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.01942
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.108a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.847
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             756
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.857
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            2021
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.857
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.407
_diffrn_reflns_theta_min         3.224
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      420.00(16)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.857
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -18.00  25.00   0.50    3.00    --   -5.29 -99.00 -30.00   86
  2  ω    -14.00  13.00   0.50    3.00    --   -5.29 -99.00 -60.00   54
  3  ω     18.00  75.00   0.50    3.00    --    5.13  52.00 109.00  114
;
_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      0.0202054000
_diffrn_orient_matrix_UB_12      0.0579265000
_diffrn_orient_matrix_UB_13      0.0236217000
_diffrn_orient_matrix_UB_21      -0.1055793000
_diffrn_orient_matrix_UB_22      0.0425955000
_diffrn_orient_matrix_UB_23      -0.0008654000
_diffrn_orient_matrix_UB_31      -0.0380288000
_diffrn_orient_matrix_UB_32      -0.0885207000
_diffrn_orient_matrix_UB_33      0.0150775000
_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                264
_reflns_number_total             421
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.160
_refine_diff_density_min         -0.827
_refine_diff_density_rms         0.214
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     36
_refine_ls_number_reflns         421
_refine_ls_number_restraints     66
_refine_ls_R_factor_all          0.0951
_refine_ls_R_factor_gt           0.0549
_refine_ls_restrained_S_all      0.949
_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)+(0.1155P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1547
_refine_ls_wR_factor_ref         0.1721
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 C9-C6 = C9-C7 = C6-C5
 1.54 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
C5 \\sim C6 \\sim C9 \\sim C7: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.01 within 2A
C5 \\sim C5A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01
within 2A
Uanis(C9) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C7) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 C6, C5, C9, C7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C5, C5A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Others
 Fixed Sof: C5(0.25) C5A(0.25)
;
_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 0.500000 0.500000 0.500000 0.0928(2) Uani 1 16 d S T P . .
Br02 Br 0.500000 0.000000 0.500000 0.1235(5) Uani 1 8 d S T P . .
Br00 Br 0.500000 0.500000 0.61545(11) 0.2120(16) Uani 1 8 d S T P . .
C5 C 1.064(3) 0.064(3) 0.7247(6) 0.275(2) Uani 0.5 2 d DS TU P A 1
C6 C 1.000000 0.230(2) 0.6830(4) 0.272(2) Uani 1 2 d DS TU P . .
C7 C 1.000000 0.000000 0.5839(8) 0.267(3) Uani 1 8 d DS TU P . .
C9 C 1.000000 0.187(2) 0.6223(4) 0.267(2) Uani 1 2 d DS TU P A .
C5A C 1.226(6) 0.226(6) 0.701(3) 0.274(4) Uani 0.5 2 d S TU P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb01 Br02 3.1114(3) . ?
Pb01 Br02 3.1114(3) 3_655 ?
Pb01 Br02 3.1114(3) 1_565 ?
Pb01 Br02 3.1114(3) 3 ?
Pb01 Br00 2.918(3) 17_666 ?
Pb01 Br00 2.918(3) . ?
C5 C5 0.80(4) 3_645 ?
C5 C5 1.12(6) 2_755 ?
C5 C5 0.80(4) 4_665 ?
C5 C6 1.529(14) . ?
C5 C6 1.529(14) 4_665 ?
C6 C6 2.027(19) 4_665 ?
C6 C6 2.027(19) 3_645 ?
C6 C9 1.558(12) . ?
C6 C5A 1.48(4) . ?
C6 C5A 1.48(4) 3_645 ?
C7 C9 1.516(14) 4_665 ?
C7 C9 1.516(14) 3_645 ?
C7 C9 1.516(14) 2_755 ?
C7 C9 1.516(14) . ?
C9 C9 1.65(2) 3_645 ?
C9 C9 1.65(2) 4_665 ?

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 180.0 . 1_565 ?
Br02 Pb01 Br02 90.0 1_565 3_655 ?
Br02 Pb01 Br02 90.0 . 3_655 ?
Br02 Pb01 Br02 90.0 . 3 ?
Br02 Pb01 Br02 90.0 1_565 3 ?
Br02 Pb01 Br02 180.0 3 3_655 ?
Br00 Pb01 Br02 90.0 17_666 3 ?
Br00 Pb01 Br02 90.0 17_666 3_655 ?
Br00 Pb01 Br02 90.0 . 1_565 ?
Br00 Pb01 Br02 90.0 . 3 ?
Br00 Pb01 Br02 90.0 17_666 1_565 ?
Br00 Pb01 Br02 90.0 17_666 . ?
Br00 Pb01 Br02 90.0 . . ?
Br00 Pb01 Br02 90.0 . 3_655 ?
Br00 Pb01 Br00 180.0 17_666 . ?
Pb01 Br02 Pb01 180.0 1_545 . ?
C5 C5 C5 45.001(10) 4_665 2_755 ?
C5 C5 C5 90.001(1) 4_665 3_645 ?
C5 C5 C5 45.001(10) 3_645 2_755 ?
C5 C5 C6 132.6(10) 4_665 . ?
C5 C5 C6 132.6(10) 3_645 4_665 ?
C5 C5 C6 74.9(9) 4_665 4_665 ?
C5 C5 C6 74.9(9) 3_645 . ?
C5 C5 C6 107.2(11) 2_755 4_665 ?
C5 C5 C6 107.2(11) 2_755 . ?
C6 C5 C6 83.0(10) . 4_665 ?
C5 C6 C5 30.1(18) . 3_645 ?
C5 C6 C6 48.5(5) 3_645 3_645 ?
C5 C6 C6 48.5(5) . 4_665 ?
C5 C6 C6 72.8(11) 3_645 4_665 ?
C5 C6 C6 72.8(11) . 3_645 ?
C5 C6 C9 124.1(12) . . ?
C5 C6 C9 124.1(12) 3_645 . ?
C6 C6 C6 89.999(5) 3_645 4_665 ?
C9 C6 C6 83.0(5) . 4_665 ?
C9 C6 C6 83.0(5) . 3_645 ?
C5A C6 C5 91(2) . 3_645 ?
C5A C6 C5 62(2) 3_645 3_645 ?
C5A C6 C6 46.7(15) 3_645 3_645 ?
C5A C6 C6 131.2(17) . 3_645 ?
C5A C6 C9 107(2) 3_645 . ?
C5A C6 C9 107(2) . . ?
C5A C6 C5A 144(5) 3_645 . ?
C9 C7 C9 65.8(8) 2_755 3_645 ?
C9 C7 C9 65.8(8) 4_665 2_755 ?
C9 C7 C9 100.4(15) 4_665 3_645 ?
C9 C7 C9 65.8(8) . 4_665 ?
C9 C7 C9 100.4(15) . 2_755 ?
C9 C7 C9 65.8(8) . 3_645 ?
C6 C9 C9 97.0(5) . 3_645 ?
C6 C9 C9 97.0(5) . 4_665 ?
C7 C9 C6 139.7(13) . . ?
C7 C9 C9 57.1(4) . 3_645 ?
C7 C9 C9 57.1(4) . 4_665 ?
C9 C9 C9 90.001(6) 3_645 4_665 ?
C6 C5A C6 87(3) . 4_665 ?

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
C5 C5 C6 C5 75.6(6) 4_665 . . 3_645 ?
C5 C5 C6 C5 31.8(4) 2_755 . . 3_645 ?
C5 C5 C6 C6 -62.0(6) 4_665 . . 4_665 ?
C5 C5 C6 C6 -105.9(11) 2_755 . . 4_665 ?
C5 C5 C6 C6 -137.7(8) 3_645 . . 4_665 ?
C5 C5 C6 C6 43.8(7) 4_665 . . 3_645 ?
C5 C5 C6 C6 -31.8(4) 3_645 . . 3_645 ?
C5 C5 C6 C6 -0.001(3) 2_755 . . 3_645 ?
C5 C5 C6 C9 -68.7(7) 2_755 . . . ?
C5 C5 C6 C9 -100.5(9) 3_645 . . . ?
C5 C5 C6 C9 -24.9(14) 4_665 . . . ?
C5 C6 C9 C7 -18.3(12) 3_645 . . . ?
C5 C6 C9 C7 18.3(12) . . . . ?
C5 C6 C9 C9 63.7(12) . . . 3_645 ?
C5 C6 C9 C9 -63.7(12) 3_645 . . 4_665 ?
C5 C6 C9 C9 -27.1(12) . . . 4_665 ?
C5 C6 C9 C9 27.1(12) 3_645 . . 3_645 ?
C6 C5 C6 C5 137.7(8) 4_665 . . 3_645 ?
C6 C5 C6 C6 105.9(11) 4_665 . . 3_645 ?
C6 C5 C6 C9 37.2(17) 4_665 . . . ?
C6 C6 C9 C7 -45.43(7) 3_645 . . . ?
C6 C6 C9 C7 45.43(6) 4_665 . . . ?
C6 C6 C9 C9 -0.001(7) 4_665 . . 4_665 ?
C6 C6 C9 C9 -90.87(12) 3_645 . . 4_665 ?
C6 C6 C9 C9 90.87(12) 4_665 . . 3_645 ?
C6 C6 C9 C9 0.001(1) 3_645 . . 3_645 ?
C6 C6 C5A C6 34(4) 3_645 . . 4_665 ?
C9 C6 C5A C6 -62(3) . . . 4_665 ?
C9 C7 C9 C6 0.000(10) 2_755 . . . ?
C9 C7 C9 C6 -57.4(4) 4_665 . . . ?
C9 C7 C9 C6 57.4(4) 3_645 . . . ?
C9 C7 C9 C9 114.8(8) 3_645 . . 4_665 ?
C9 C7 C9 C9 -57.4(4) 2_755 . . 3_645 ?
C9 C7 C9 C9 -114.8(8) 4_665 . . 3_645 ?
C9 C7 C9 C9 57.4(4) 2_755 . . 4_665 ?
C5A C6 C9 C7 85.7(18) . . . . ?
C5A C6 C9 C7 -85.7(18) 3_645 . . . ?
C5A C6 C9 C9 131.1(17) . . . 3_645 ?
C5A C6 C9 C9 -40.2(18) 3_645 . . 3_645 ?
C5A C6 C9 C9 -131.1(17) 3_645 . . 4_665 ?
C5A C6 C9 C9 40.2(18) . . . 4_665 ?
C5A C6 C5A C6 104(5) 3_645 . . 4_665 ?

_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 15.403
_oxdiff_exptl_absorpt_empirical_full_min 0.262

# start Validation Reply Form
_vrf_PLAT242_hxq-211027-2-420k-2st_auto 
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of       Pb01 Check 
RESPONSE: These alerts are generated because there is a large amount of disorder
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_yh_211207_2_299k_auto
_database_code_depnum_ccdc_archive 'CCDC 2195162'
loop_
_audit_author_name
_audit_author_address
'Zhong-Xia Wang'
;Nanchang University
China
;
_audit_update_record             
;
2022-08-05 deposited with the CCDC.	2023-12-03 downloaded from the CCDC.
;
_audit_creation_date             2022-04-16
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br16 Pb5, 5.922(C5 H11 F N)'
_chemical_formula_sum            'C30 H62 Br16 F6 N6 Pb5'
_chemical_formula_weight         2935.36
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H N F Pb Br'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   12.5612(5)
_cell_length_b                   32.8585(16)
_cell_length_c                   8.1977(3)
_cell_angle_alpha                90
_cell_angle_beta                 104.943(4)
_cell_angle_gamma                90
_cell_volume                     3269.1(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7862
_cell_measurement_temperature    298.95(10)
_cell_measurement_theta_max      30.8880
_cell_measurement_theta_min      1.8340
_shelx_estimated_absorpt_T_max   0.805
_shelx_estimated_absorpt_T_min   0.550
_exptl_absorpt_coefficient_mu    22.655
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52061
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.108a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.982
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2616
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            23022
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.086
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      298.95(10)
_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 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -69.00  17.00   0.50    1.00    --    5.05 -19.00 -60.00  172
  2  ω    -17.00  11.00   0.50    1.00    --   -5.21 -99.00  30.00   56
  3  ω    -65.00  18.00   0.50    1.00    --    5.05 -57.00  60.00  166
  4  ω      1.00  27.00   0.50    1.00    --    5.05  57.00 120.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0000176000
_diffrn_orient_matrix_UB_12      -0.0208090000
_diffrn_orient_matrix_UB_13      0.0230480000
_diffrn_orient_matrix_UB_21      0.0569774000
_diffrn_orient_matrix_UB_22      -0.0012882000
_diffrn_orient_matrix_UB_23      0.0039441000
_diffrn_orient_matrix_UB_31      0.0129843000
_diffrn_orient_matrix_UB_32      0.0056035000
_diffrn_orient_matrix_UB_33      0.0864302000
_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                5140
_reflns_number_total             6419
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         1.818
_refine_diff_density_min         -1.487
_refine_diff_density_rms         0.180
_refine_ls_extinction_coef       0.00067(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     288
_refine_ls_number_reflns         6419
_refine_ls_number_restraints     49
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0354
_refine_ls_restrained_S_all      1.042
_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)+(0.0159P)²+16.1333P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0658
_refine_ls_wR_factor_ref         0.0692
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
2. Restrained distances
 F12A-C13
 1.43 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N3 \\sim C15 \\sim C11 \\sim C14 \\sim C12 \\sim C13 \\sim F12A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.01 within 2A
C12 \\sim C13 \\sim F12A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.01 within 2A
4. Others
 Sof(N3)=Sof(H3A)=Sof(H3B)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(C15)=Sof(H15A)=
 Sof(H15B)=Sof(C13)=Sof(H13)=Sof(F12A)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(C11)=
 Sof(H11A)=Sof(H11B)=1-FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C3(H3), C10(H10), C13(H13)
5.b Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C9(H9A,H9B), C6(H6A,H6B), C1(H1C,H1D), C4(H4A,H4B), C7(H7A,H7B),
 C8(H8A,H8B), C5(H5A,H5B), C2(H2A,H2B), N2(H2C,H2D), N3(H3A,H3B), C14(H14A,
 H14B), C15(H15A,H15B), C12(H12A,H12B), C11(H11A,H11B)
;
_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 0.10917(2) 0.18754(2) 0.24466(3) 0.02971(9) Uani 1 1 d . . . . .
Pb2 Pb 0.28743(2) 0.08807(2) 0.37201(4) 0.03064(9) Uani 1 1 d . . . . .
Pb3 Pb 0.500000 0.000000 0.500000 0.03099(11) Uani 1 2 d S . P . .
Br5 Br 0.37492(7) 0.16969(3) 0.36860(10) 0.0365(2) Uani 1 1 d . . . . .
Br7 Br 0.45340(8) 0.07054(3) 0.70877(10) 0.0444(2) Uani 1 1 d . . . . .
Br1 Br -0.12132(7) 0.18412(4) 0.11279(11) 0.0497(3) Uani 1 1 d . . . . .
Br3 Br 0.11341(7) 0.12020(3) 0.52221(11) 0.0475(2) Uani 1 1 d . . . . .
Br4 Br 0.14821(7) 0.11503(3) 0.03352(10) 0.0452(2) Uani 1 1 d . . . . .
Br8 Br 0.45642(8) 0.05442(3) 0.19373(12) 0.0505(3) Uani 1 1 d . . . . .
Br6 Br 0.25134(8) -0.00760(3) 0.41409(12) 0.0499(2) Uani 1 1 d . . . . .
Br2 Br 0.11697(9) 0.23669(4) -0.04749(14) 0.0633(3) Uani 1 1 d . . . . .
C3 C 0.6994(8) 0.1582(4) 0.5586(13) 0.064(3) Uani 1 1 d . . . . .
H3 H 0.623101 0.164006 0.560274 0.077 Uiso 1 1 calc R U . . .
F23 F 0.7006(6) 0.1410(3) 0.4008(7) 0.093(2) Uani 1 1 d . . . . .
F1 F 0.5618(5) 0.2176(2) -0.2036(7) 0.0729(19) Uani 1 1 d . . . . .
N1 N 0.9270(6) 0.1593(2) 0.7275(9) 0.0439(19) Uani 1 1 d . . . . .
H1A H 0.925329 0.169922 0.826687 0.053 Uiso 1 1 calc R U . . .
H1B H 0.997089 0.154326 0.730442 0.053 Uiso 1 1 calc R U . . .
C9 C 0.5665(7) 0.1974(3) 0.0721(10) 0.039(2) Uani 1 1 d . . . . .
H9A H 0.645751 0.201006 0.098574 0.047 Uiso 1 1 calc R U . . .
H9B H 0.542316 0.204614 0.171504 0.047 Uiso 1 1 calc R U . . .
C6 C 0.3930(8) 0.2179(3) -0.1293(12) 0.048(2) Uani 1 1 d . . . . .
H6A H 0.363829 0.234046 -0.229949 0.058 Uiso 1 1 calc R U . . .
H6B H 0.357661 0.226948 -0.043444 0.058 Uiso 1 1 calc R U . . .
C1 C 0.8659(8) 0.1201(3) 0.7051(12) 0.051(2) Uani 1 1 d . . . . .
H1C H 0.895790 0.102545 0.801008 0.061 Uiso 1 1 calc R U . . .
H1D H 0.874732 0.106536 0.604306 0.061 Uiso 1 1 calc R U . . .
C10 C 0.5133(7) 0.2249(3) -0.0689(11) 0.043(2) Uani 1 1 d . . . . .
H10 H 0.526757 0.253220 -0.031692 0.051 Uiso 1 1 calc R U . . .
C4 C 0.7625(9) 0.1962(4) 0.5820(15) 0.067(3) Uani 1 1 d . . . . .
H4A H 0.755364 0.209427 0.684566 0.081 Uiso 1 1 calc R U . . .
H4B H 0.731700 0.214328 0.488235 0.081 Uiso 1 1 calc R U . . .
C7 C 0.3648(7) 0.1729(3) -0.1695(11) 0.044(2) Uani 1 1 d . . . . .
H7A H 0.285576 0.169178 -0.197634 0.053 Uiso 1 1 calc R U . . .
H7B H 0.391029 0.164603 -0.265835 0.053 Uiso 1 1 calc R U . . .
C8 C 0.5396(7) 0.1539(3) 0.0300(12) 0.046(2) Uani 1 1 d . . . . .
H8A H 0.571790 0.137015 0.127400 0.055 Uiso 1 1 calc R U . . .
H8B H 0.570690 0.145590 -0.061541 0.055 Uiso 1 1 calc R U . . .
C5 C 0.8828(8) 0.1896(3) 0.5934(12) 0.051(2) Uani 1 1 d . . . . .
H5A H 0.891657 0.179724 0.486107 0.061 Uiso 1 1 calc R U . . .
H5B H 0.922673 0.214993 0.619662 0.061 Uiso 1 1 calc R U . . .
C2 C 0.7465(7) 0.1274(3) 0.6896(12) 0.051(3) Uani 1 1 d . . . . .
H2A H 0.706590 0.102065 0.661478 0.061 Uiso 1 1 calc R U . . .
H2B H 0.737180 0.136618 0.797543 0.061 Uiso 1 1 calc R U . . .
N2 N 0.4176(6) 0.1479(2) -0.0210(8) 0.0401(17) Uani 1 1 d . . . . .
H2C H 0.402616 0.121784 -0.045009 0.048 Uiso 1 1 calc R U . . .
H2D H 0.389706 0.154568 0.064828 0.048 Uiso 1 1 calc R U . . .
N3 N 0.7208(10) 0.0037(4) 0.1369(17) 0.102(4) Uani 0.961(12) 1 d . U P A 2
H3A H 0.695797 0.003485 0.229060 0.122 Uiso 0.961(12) 1 calc R U P A 2
H3B H 0.668724 -0.007310 0.053953 0.122 Uiso 0.961(12) 1 calc R U P A 2
C14 C 0.9126(12) -0.0028(6) 0.237(2) 0.101(4) Uani 0.961(12) 1 d . U P A 2
H14A H 0.968857 -0.018785 0.205367 0.121 Uiso 0.961(12) 1 calc R U P A 2
H14B H 0.926819 -0.004119 0.359334 0.121 Uiso 0.961(12) 1 calc R U P A 2
C15 C 0.8095(14) -0.0206(5) 0.166(2) 0.103(4) Uani 0.961(12) 1 d . U P A 2
H15A H 0.812102 -0.032786 0.058932 0.123 Uiso 0.961(12) 1 calc R U P A 2
H15B H 0.798796 -0.042442 0.239166 0.123 Uiso 0.961(12) 1 calc R U P A 2
C13 C 0.9242(14) 0.0416(6) 0.1870(18) 0.111(4) Uani 0.961(12) 1 d D U P A 2
H13 H 0.989866 0.054396 0.259972 0.133 Uiso 0.961(12) 1 calc R U P A 2
F12A F 0.9225(7) 0.0454(3) 0.0061(9) 0.109(3) Uani 0.961(12) 1 d D U P A 2
C12 C 0.8381(15) 0.0649(6) 0.167(2) 0.118(4) Uani 0.961(12) 1 d . U P A 2
H12A H 0.848545 0.088094 0.099569 0.142 Uiso 0.961(12) 1 calc R U P A 2
H12B H 0.836149 0.075112 0.276891 0.142 Uiso 0.961(12) 1 calc R U P A 2
C11 C 0.7339(13) 0.0479(6) 0.091(2) 0.105(4) Uani 0.961(12) 1 d . U P A 2
H11A H 0.720783 0.049940 -0.030953 0.126 Uiso 0.961(12) 1 calc R U P A 2
H11B H 0.677898 0.064037 0.123106 0.126 Uiso 0.961(12) 1 calc R U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br1 2.8194(9) . ?
Pb1 Br3 3.1643(10) . ?
Pb1 Br4 3.0577(10) . ?
Pb1 Br2 2.9111(10) . ?
Pb1 Br2 3.0044(11) 4_566 ?
Pb2 Br5 2.9012(9) . ?
Pb2 Br7 3.0547(9) . ?
Pb2 Br3 2.9659(9) . ?
Pb2 Br4 3.0067(9) . ?
Pb2 Br8 3.0764(10) . ?
Pb2 Br6 3.2074(11) . ?
Pb3 Br7 3.0267(9) 3_656 ?
Pb3 Br7 3.0266(9) . ?
Pb3 Br8 3.0154(9) . ?
Pb3 Br8 3.0154(9) 3_656 ?
Pb3 Br6 3.0298(9) 3_656 ?
Pb3 Br6 3.0298(9) . ?
C3 H3 0.9800 . ?
C3 F23 1.417(12) . ?
C3 C4 1.465(16) . ?
C3 C2 1.483(15) . ?
F1 C10 1.413(10) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C1 1.485(12) . ?
N1 C5 1.481(12) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.484(12) . ?
C9 C8 1.489(13) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C10 1.483(12) . ?
C6 C7 1.535(13) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C1 C2 1.491(13) . ?
C10 H10 0.9800 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C5 1.506(14) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 N2 1.477(11) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 N2 1.494(11) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
N2 H2C 0.8900 . ?
N2 H2D 0.8900 . ?
N3 H3A 0.8900 . ?
N3 H3B 0.8900 . ?
N3 C15 1.341(19) . ?
N3 C11 1.52(2) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C15 1.41(2) . ?
C14 C13 1.53(2) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C13 H13 0.9800 . ?
C13 F12A 1.483(13) . ?
C13 C12 1.30(2) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 C11 1.41(2) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br1 Pb1 Br3 94.19(3) . . ?
Br1 Pb1 Br4 92.90(3) . . ?
Br1 Pb1 Br2 97.50(3) . 4_566 ?
Br1 Pb1 Br2 87.46(3) . . ?
Br4 Pb1 Br3 83.50(3) . . ?
Br2 Pb1 Br3 168.98(3) . . ?
Br2 Pb1 Br3 100.35(3) 4_566 . ?
Br2 Pb1 Br4 85.54(3) . . ?
Br2 Pb1 Br4 168.58(3) 4_566 . ?
Br2 Pb1 Br2 90.211(12) . 4_566 ?
Br5 Pb2 Br7 90.64(3) . . ?
Br5 Pb2 Br3 89.80(3) . . ?
Br5 Pb2 Br4 81.39(3) . . ?
Br5 Pb2 Br8 91.04(3) . . ?
Br5 Pb2 Br6 166.28(3) . . ?
Br7 Pb2 Br8 88.16(3) . . ?
Br7 Pb2 Br6 78.49(3) . . ?
Br3 Pb2 Br7 95.52(3) . . ?
Br3 Pb2 Br4 87.86(3) . . ?
Br3 Pb2 Br8 176.22(3) . . ?
Br3 Pb2 Br6 99.47(3) . . ?
Br4 Pb2 Br7 171.34(3) . . ?
Br4 Pb2 Br8 88.61(3) . . ?
Br4 Pb2 Br6 108.87(3) . . ?
Br8 Pb2 Br6 80.38(3) . . ?
Br7 Pb3 Br7 180.0 . 3_656 ?
Br7 Pb3 Br6 98.25(3) . 3_656 ?
Br7 Pb3 Br6 81.75(3) . . ?
Br7 Pb3 Br6 81.75(3) 3_656 3_656 ?
Br7 Pb3 Br6 98.25(3) 3_656 . ?
Br8 Pb3 Br7 90.20(3) . 3_656 ?
Br8 Pb3 Br7 89.80(3) 3_656 3_656 ?
Br8 Pb3 Br7 90.19(3) 3_656 . ?
Br8 Pb3 Br7 89.81(3) . . ?
Br8 Pb3 Br8 180.00(3) . 3_656 ?
Br8 Pb3 Br6 84.28(3) 3_656 3_656 ?
Br8 Pb3 Br6 95.72(3) . 3_656 ?
Br8 Pb3 Br6 84.28(3) . . ?
Br8 Pb3 Br6 95.72(3) 3_656 . ?
Br6 Pb3 Br6 180.0 3_656 . ?
Pb3 Br7 Pb2 79.62(2) . . ?
Pb2 Br3 Pb1 80.09(2) . . ?
Pb2 Br4 Pb1 81.21(2) . . ?
Pb3 Br8 Pb2 79.45(2) . . ?
Pb3 Br6 Pb2 77.20(2) . . ?
Pb1 Br2 Pb1 157.41(5) . 4_565 ?
F23 C3 H3 109.3 . . ?
F23 C3 C4 109.2(10) . . ?
F23 C3 C2 106.9(10) . . ?
C4 C3 H3 109.3 . . ?
C4 C3 C2 112.6(9) . . ?
C2 C3 H3 109.3 . . ?
H1A N1 H1B 107.6 . . ?
C1 N1 H1A 108.7 . . ?
C1 N1 H1B 108.7 . . ?
C5 N1 H1A 108.7 . . ?
C5 N1 H1B 108.7 . . ?
C5 N1 C1 114.0(7) . . ?
H9A C9 H9B 107.9 . . ?
C10 C9 H9A 109.2 . . ?
C10 C9 H9B 109.2 . . ?
C8 C9 H9A 109.2 . . ?
C8 C9 H9B 109.2 . . ?
C8 C9 C10 112.0(7) . . ?
H6A C6 H6B 107.9 . . ?
C10 C6 H6A 109.1 . . ?
C10 C6 H6B 109.1 . . ?
C10 C6 C7 112.3(8) . . ?
C7 C6 H6A 109.1 . . ?
C7 C6 H6B 109.1 . . ?
N1 C1 H1C 109.6 . . ?
N1 C1 H1D 109.6 . . ?
N1 C1 C2 110.3(8) . . ?
H1C C1 H1D 108.1 . . ?
C2 C1 H1C 109.6 . . ?
C2 C1 H1D 109.6 . . ?
F1 C10 C9 107.9(7) . . ?
F1 C10 C6 108.7(7) . . ?
F1 C10 H10 109.3 . . ?
C9 C10 H10 109.3 . . ?
C6 C10 C9 112.4(8) . . ?
C6 C10 H10 109.3 . . ?
C3 C4 H4A 109.1 . . ?
C3 C4 H4B 109.1 . . ?
C3 C4 C5 112.6(10) . . ?
H4A C4 H4B 107.8 . . ?
C5 C4 H4A 109.1 . . ?
C5 C4 H4B 109.1 . . ?
C6 C7 H7A 109.8 . . ?
C6 C7 H7B 109.8 . . ?
H7A C7 H7B 108.3 . . ?
N2 C7 C6 109.2(7) . . ?
N2 C7 H7A 109.8 . . ?
N2 C7 H7B 109.8 . . ?
C9 C8 H8A 109.6 . . ?
C9 C8 H8B 109.6 . . ?
C9 C8 N2 110.2(7) . . ?
H8A C8 H8B 108.1 . . ?
N2 C8 H8A 109.6 . . ?
N2 C8 H8B 109.6 . . ?
N1 C5 C4 108.8(8) . . ?
N1 C5 H5A 109.9 . . ?
N1 C5 H5B 109.9 . . ?
C4 C5 H5A 109.9 . . ?
C4 C5 H5B 109.9 . . ?
H5A C5 H5B 108.3 . . ?
C3 C2 C1 112.1(8) . . ?
C3 C2 H2A 109.2 . . ?
C3 C2 H2B 109.2 . . ?
C1 C2 H2A 109.2 . . ?
C1 C2 H2B 109.2 . . ?
H2A C2 H2B 107.9 . . ?
C7 N2 C8 111.6(7) . . ?
C7 N2 H2C 109.3 . . ?
C7 N2 H2D 109.3 . . ?
C8 N2 H2C 109.3 . . ?
C8 N2 H2D 109.3 . . ?
H2C N2 H2D 108.0 . . ?
H3A N3 H3B 107.1 . . ?
C15 N3 H3A 107.7 . . ?
C15 N3 H3B 107.7 . . ?
C15 N3 C11 118.3(12) . . ?
C11 N3 H3A 107.7 . . ?
C11 N3 H3B 107.7 . . ?
H14A C14 H14B 107.5 . . ?
C15 C14 H14A 108.5 . . ?
C15 C14 H14B 108.5 . . ?
C15 C14 C13 115.1(15) . . ?
C13 C14 H14A 108.5 . . ?
C13 C14 H14B 108.5 . . ?
N3 C15 C14 117.4(16) . . ?
N3 C15 H15A 108.0 . . ?
N3 C15 H15B 108.0 . . ?
C14 C15 H15A 108.0 . . ?
C14 C15 H15B 108.0 . . ?
H15A C15 H15B 107.2 . . ?
C14 C13 H13 111.5 . . ?
F12A C13 C14 111.9(14) . . ?
F12A C13 H13 111.5 . . ?
C12 C13 C14 117.4(15) . . ?
C12 C13 H13 111.5 . . ?
C12 C13 F12A 91.4(14) . . ?
C13 C12 H12A 107.8 . . ?
C13 C12 H12B 107.8 . . ?
C13 C12 C11 118.2(19) . . ?
H12A C12 H12B 107.1 . . ?
C11 C12 H12A 107.8 . . ?
C11 C12 H12B 107.8 . . ?
N3 C11 H11A 108.7 . . ?
N3 C11 H11B 108.7 . . ?
C12 C11 N3 114.4(15) . . ?
C12 C11 H11A 108.7 . . ?
C12 C11 H11B 108.7 . . ?
H11A C11 H11B 107.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 C4 C5 N1 -54.1(12) . . . . ?
F23 C3 C4 C5 -64.5(11) . . . . ?
F23 C3 C2 C1 67.1(11) . . . . ?
N1 C1 C2 C3 52.0(11) . . . . ?
C9 C8 N2 C7 59.4(9) . . . . ?
C6 C7 N2 C8 -57.7(10) . . . . ?
C1 N1 C5 C4 55.4(11) . . . . ?
C10 C9 C8 N2 -55.6(10) . . . . ?
C10 C6 C7 N2 53.8(10) . . . . ?
C4 C3 C2 C1 -52.8(13) . . . . ?
C7 C6 C10 F1 67.8(10) . . . . ?
C7 C6 C10 C9 -51.6(11) . . . . ?
C8 C9 C10 F1 -67.2(9) . . . . ?
C8 C9 C10 C6 52.6(10) . . . . ?
C5 N1 C1 C2 -55.2(10) . . . . ?
C2 C3 C4 C5 54.1(13) . . . . ?
C14 C13 C12 C11 -38(2) . . . . ?
C15 N3 C11 C12 -33(2) . . . . ?
C15 C14 C13 F12A -67.9(18) . . . . ?
C15 C14 C13 C12 36(2) . . . . ?
C13 C14 C15 N3 -33(2) . . . . ?
C13 C12 C11 N3 36(2) . . . . ?
F12A C13 C12 C11 77.3(17) . . . . ?
C11 N3 C15 C14 33(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.752
_oxdiff_exptl_absorpt_empirical_full_min 0.627
####################################################################### 
# 
# 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_hxq-211027-2-293k_2st-auto
_database_code_depnum_ccdc_archive 'CCDC 2195165'
loop_
_audit_author_name
_audit_author_address
'Zhong-Xia Wang'
;Nanchang University
China
;
_audit_update_record             
;
2022-08-05 deposited with the CCDC.	2023-12-03 downloaded from the CCDC.
;
_audit_creation_date             2022-01-18
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br4 Pb, 2(C5 H10 F2 N)'
_chemical_formula_sum            'C10 H20 Br4 F4 N2 Pb'
_chemical_formula_weight         771.11
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H  N F Pb Br'
_chemical_oxdiff_usercomment     \
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'
F F 0.0171 0.0103 '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           41
_space_group_name_H-M_alt        'A e a 2'
_space_group_name_Hall           'A 2 -2ac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y, z+1/2'
'x+1/2, -y, z+1/2'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1'
'x+1/2, -y+1/2, z+1'

_cell_length_a                   8.8355(8)
_cell_length_b                   25.181(3)
_cell_length_c                   8.7566(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1948.2(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1883
_cell_measurement_temperature    293(11)
_cell_measurement_theta_max      26.5100
_cell_measurement_theta_min      3.2430
_shelx_estimated_absorpt_T_max   0.729
_shelx_estimated_absorpt_T_min   0.551
_exptl_absorpt_coefficient_mu    16.892
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.13741
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.108a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.629
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0774
_diffrn_reflns_av_unetI/netI     0.0726
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.816
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5123
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.737
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.674
_diffrn_reflns_theta_min         2.816
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293(11)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.816
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -36.00 -10.00   0.50    2.00    --    5.05 -81.00 116.00   52
  2  ω    -19.00  35.00   0.50    2.00    --    5.05 -98.00  22.00  108
  3  ω    -15.00  24.00   0.50    2.00    --   -5.21 -99.00-120.00   78
  4  ω    -17.00  33.00   0.50    2.00    --    5.05 -99.00-180.00  100
;
_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      -0.0179960000
_diffrn_orient_matrix_UB_12      -0.0240392000
_diffrn_orient_matrix_UB_13      0.0381503000
_diffrn_orient_matrix_UB_21      -0.0738100000
_diffrn_orient_matrix_UB_22      0.0007082000
_diffrn_orient_matrix_UB_23      -0.0317816000
_diffrn_orient_matrix_UB_31      0.0259628000
_diffrn_orient_matrix_UB_32      -0.0146267000
_diffrn_orient_matrix_UB_33      -0.0640596000
_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         0.698
_reflns_Friedel_fraction_full    0.917
_reflns_Friedel_fraction_max     0.646
_reflns_number_gt                1239
_reflns_number_total             2226
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         1.933
_refine_diff_density_min         -2.065
_refine_diff_density_rms         0.271
_refine_ls_abs_structure_details 
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.07(5)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     96
_refine_ls_number_reflns         2226
_refine_ls_number_restraints     58
_refine_ls_R_factor_all          0.1243
_refine_ls_R_factor_gt           0.0815
_refine_ls_restrained_S_all      1.031
_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)+(0.1760P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2505
_refine_ls_wR_factor_ref         0.2801
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
2. Restrained distances
 C3-C12 = C3-C2 = C4-C2 = C4-C1
 1.54 with sigma of 0.02
 F7-C2 = F4-C2
 1.4 with sigma of 0.02
 N6-C12 = N6-C1
 1.46 with sigma of 0.02
 F4-F7
 2.15 with sigma of 0.03
3. Uiso/Uaniso restraints and constraints
Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F4) \\sim Ueq, Uanis(F7) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C3) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(N6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C4(H4A,H4B), N6(H6A,H6B), C12(H12A,H12B)
;
_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 -0.500000 0.000000 -1.03633(2) 0.07006(17) Uani 1 2 d S T P . .
Br2 Br -0.2374(3) 0.00400(5) -1.2822(3) 0.1002(4) Uani 1 1 d . . . . .
Br3 Br -0.4629(2) -0.11644(7) -1.0262(4) 0.1082(5) Uani 1 1 d . . . . .
C1 C -0.4815(12) -0.1009(7) -0.5158(17) 0.127(5) Uani 1 1 d D U . . .
H1A H -0.498621 -0.063001 -0.524098 0.152 Uiso 1 1 calc R U . . .
H1B H -0.411054 -0.106533 -0.432364 0.152 Uiso 1 1 calc R U . . .
C3 C -0.5216(14) -0.2124(7) -0.6251(17) 0.138(5) Uani 1 1 d D U . . .
H3A H -0.593264 -0.214183 -0.708855 0.166 Uiso 1 1 calc R U . . .
H3B H -0.487951 -0.248050 -0.600564 0.166 Uiso 1 1 calc R U . . .
C4 C -0.6285(14) -0.1271(4) -0.475(2) 0.112(4) Uani 1 1 d D U . . .
H4A H -0.707692 -0.117142 -0.546663 0.134 Uiso 1 1 calc R U . . .
H4B H -0.659953 -0.117735 -0.372761 0.134 Uiso 1 1 calc R U . . .
N6 N -0.4096(17) -0.1194(4) -0.6583(13) 0.113(4) Uani 1 1 d D U . . .
H6A H -0.466423 -0.109334 -0.736999 0.136 Uiso 1 1 calc R U . . .
H6B H -0.319851 -0.103755 -0.667711 0.136 Uiso 1 1 calc R U . . .
F7 F -0.7287(12) -0.2122(5) -0.497(2) 0.217(5) Uani 1 1 d D U . . .
C12 C -0.3885(15) -0.1770(4) -0.665(2) 0.141(5) Uani 1 1 d D U . . .
H12A H -0.305472 -0.186156 -0.597875 0.169 Uiso 1 1 calc R U . . .
H12B H -0.356831 -0.185902 -0.768406 0.169 Uiso 1 1 calc R U . . .
C2 C -0.5918(13) -0.1860(4) -0.4874(13) 0.144(5) Uani 1 1 d D U . . .
F4 F -0.5206(16) -0.2049(10) -0.3581(16) 0.258(9) Uani 1 1 d D 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 Br2 3.060(3) 3_455 ?
Pb1 Br2 3.167(3) 2_455 ?
Pb1 Br2 3.060(3) 4_455 ?
Pb1 Br2 3.167(3) . ?
Pb1 Br3 2.9516(17) . ?
Pb1 Br3 2.9516(17) 2_455 ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C4 1.498(15) . ?
C1 N6 1.475(16) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C12 1.517(16) . ?
C3 C2 1.510(16) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C2 1.523(13) . ?
N6 H6A 0.8900 . ?
N6 H6B 0.8900 . ?
N6 C12 1.463(13) . ?
F7 C2 1.381(14) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C2 F4 1.379(16) . ?

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
Br2 Pb1 Br2 86.68(11) 3_455 4_455 ?
Br2 Pb1 Br2 94.34(10) 2_455 . ?
Br2 Pb1 Br2 176.16(11) 4_455 . ?
Br2 Pb1 Br2 176.16(11) 3_455 2_455 ?
Br2 Pb1 Br2 89.493(9) 4_455 2_455 ?
Br2 Pb1 Br2 89.492(8) 3_455 . ?
Br3 Pb1 Br2 94.03(6) . 2_455 ?
Br3 Pb1 Br2 94.02(6) 2_455 . ?
Br3 Pb1 Br2 86.26(6) 2_455 4_455 ?
Br3 Pb1 Br2 88.32(6) 2_455 2_455 ?
Br3 Pb1 Br2 91.23(6) . 4_455 ?
Br3 Pb1 Br2 86.26(6) . 3_455 ?
Br3 Pb1 Br2 91.23(6) 2_455 3_455 ?
Br3 Pb1 Br2 88.32(6) . . ?
Br3 Pb1 Br3 176.55(14) . 2_455 ?
Pb1 Br2 Pb1 174.66(8) 3_454 . ?
H1A C1 H1B 107.4 . . ?
C4 C1 H1A 108.4 . . ?
C4 C1 H1B 108.4 . . ?
N6 C1 H1A 108.4 . . ?
N6 C1 H1B 108.4 . . ?
N6 C1 C4 115.7(13) . . ?
H3A C3 H3B 108.9 . . ?
C12 C3 H3A 110.9 . . ?
C12 C3 H3B 110.9 . . ?
C2 C3 H3A 110.9 . . ?
C2 C3 H3B 110.9 . . ?
C2 C3 C12 104.3(12) . . ?
C1 C4 H4A 111.1 . . ?
C1 C4 H4B 111.1 . . ?
C1 C4 C2 103.1(11) . . ?
H4A C4 H4B 109.1 . . ?
C2 C4 H4A 111.1 . . ?
C2 C4 H4B 111.1 . . ?
C1 N6 H6A 108.8 . . ?
C1 N6 H6B 108.8 . . ?
H6A N6 H6B 107.7 . . ?
C12 N6 C1 113.8(12) . . ?
C12 N6 H6A 108.8 . . ?
C12 N6 H6B 108.8 . . ?
C3 C12 H12A 107.8 . . ?
C3 C12 H12B 107.8 . . ?
N6 C12 C3 118.2(12) . . ?
N6 C12 H12A 107.8 . . ?
N6 C12 H12B 107.8 . . ?
H12A C12 H12B 107.1 . . ?
C3 C2 C4 124.8(12) . . ?
F7 C2 C3 95.8(11) . . ?
F7 C2 C4 106.5(10) . . ?
F4 C2 C3 108.4(12) . . ?
F4 C2 C4 112.1(14) . . ?
F4 C2 F7 106.6(12) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C4 C2 C3 -53.0(17) . . . . ?
C1 C4 C2 F7 -162.5(13) . . . . ?
C1 C4 C2 F4 81.3(15) . . . . ?
C1 N6 C12 C3 48.3(19) . . . . ?
C4 C1 N6 C12 -53.5(17) . . . . ?
N6 C1 C4 C2 50.7(17) . . . . ?
C12 C3 C2 C4 48.1(16) . . . . ?
C12 C3 C2 F7 162.7(12) . . . . ?
C12 C3 C2 F4 -87.6(15) . . . . ?
C2 C3 C12 N6 -41.6(18) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.763
_oxdiff_exptl_absorpt_empirical_full_min 0.421
####################################################################### 
# 
# 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_cmca
_database_code_depnum_ccdc_archive 'CCDC 2195163'
loop_
_audit_author_name
_audit_author_address
'Zhong-Xia Wang'
;Nanchang University
China
;
_audit_update_record             
;
2022-08-05 deposited with the CCDC.	2023-12-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Br16 Pb5, 6(C5 H11 F N)'
_chemical_formula_sum            'Br16 Pb5, 6(C5 H11 F N)'
_chemical_formula_weight         2939.29

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           64
_space_group_name_H-M_alt        'C m c a'
_space_group_name_Hall           '-C 2bc 2'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y+1/2, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y-1/2, -z-1/2'
'x, -y-1/2, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y, -z-1/2'
'x+1/2, -y, z-1/2'
'-x+1/2, y+1/2, z'

_cell_length_a                   8.3832(7)
_cell_length_b                   24.1380(15)
_cell_length_c                   33.398(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6758.1(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    440(2)
_cell_measurement_reflns_used    7891
_cell_measurement_theta_min      2.3720
_cell_measurement_theta_max      75.3830

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.889
_exptl_crystal_F_000             8120
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_exptl_absorpt_coefficient_mu    21.918
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.140
_exptl_absorpt_correction_T_max  0.216
_exptl_absorpt_process_details   'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      440(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17834
_diffrn_reflns_av_unetI/netI     0.0539
_diffrn_reflns_av_R_equivalents  0.0492
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_theta_min         2.082
_diffrn_reflns_theta_max         31.112
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.803
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.803
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.803
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4640
_reflns_number_gt                2296
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0623P)²+12.0800P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4640
_refine_ls_number_parameters     193
_refine_ls_number_restraints     616
_refine_ls_R_factor_all          0.1184
_refine_ls_R_factor_gt           0.0465
_refine_ls_wR_factor_ref         0.1369
_refine_ls_wR_factor_gt          0.1147
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.007
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.001

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
C3 C 0.5000 0.7095(4) 0.1627(3) 0.1955(14) Uani 0.5 2 d DS TU P . .
H3A H 0.5922 0.7331 0.1623 0.235 Uiso 0.5 1 d R U P . .
H3B H 0.4079 0.7331 0.1623 0.235 Uiso 0.5 1 d R U P . .
N3 N 0.5000 0.7095(4) 0.1627(3) 0.1955(14) Uani 0.5 2 d S TU P . .
C4 C 0.5000 0.6808(4) 0.2009(3) 0.1975(14) Uani 0.5 2 d DS TU P . .
H4A H 0.4082 0.6932 0.2156 0.237 Uiso 0.5 1 d R U P . .
H4B H 0.5918 0.6932 0.2156 0.237 Uiso 0.5 1 d R U P . .
N4 N 0.5000 0.6808(4) 0.2009(3) 0.1975(14) Uani 0.5 2 d S TU P . .
C10 C 1.0000 0.4461(4) 0.1453(3) 0.2121(14) Uani 0.5 2 d DS TU P . .
H10A H 0.9078 0.4383 0.1292 0.255 Uiso 0.5 1 d R U P . .
H10B H 1.0922 0.4383 0.1292 0.255 Uiso 0.5 1 d R U P . .
C9 C 1.0000 0.4096(4) 0.1783(3) 0.2138(14) Uani 0.5 2 d DS TU P . .
H9A H 1.0917 0.3863 0.1750 0.257 Uiso 0.5 1 d R U P . .
H9B H 0.9083 0.3863 0.1750 0.257 Uiso 0.5 1 d R U P . .
N10 N 1.0000 0.4461(4) 0.1453(3) 0.2121(14) Uani 0.5 2 d S TU P . .
N9 N 1.0000 0.4096(4) 0.1783(3) 0.2138(14) Uani 0.5 2 d S TU P . .
C14 C 0.0000 0.3979(4) 0.9881(3) 0.2077(14) Uani 0.5 2 d DS TU P . .
H14A H 0.0918 0.4212 0.9915 0.249 Uiso 0.5 1 d R U P . .
H14B H -0.0918 0.4212 0.9915 0.249 Uiso 0.5 1 d R U P . .
C15 C 0.0000 0.3604(4) 1.0206(3) 0.2073(14) Uani 0.5 2 d DS TU P . .
H15A H -0.0922 0.3681 1.0368 0.249 Uiso 0.5 1 d R U P . .
H15B H 0.0922 0.3681 1.0368 0.249 Uiso 0.5 1 d R U P . .
N14 N 0.0000 0.3979(4) 0.9881(3) 0.2077(14) Uani 0.5 2 d S TU P . .
N15 N 0.0000 0.3604(4) 1.0206(3) 0.2073(14) Uani 0.5 2 d S TU P . .
C16 C 0.0000 0.3031(4) 1.0124(3) 0.2075(19) Uani 1 2 d DS TU P . .
H16A H -0.0917 0.2877 1.0255 0.249 Uiso 0.5 1 d R U P . .
H16B H 0.0917 0.2877 1.0255 0.249 Uiso 0.5 1 d R U P . .
C6 C 0.5000 0.5902(3) 0.1638(3) 0.2040(19) Uani 1 2 d DS TU P . .
H6A H 0.5920 0.5665 0.1640 0.245 Uiso 0.375 1 d R U P . .
H6B H 0.4080 0.5665 0.1640 0.245 Uiso 0.375 1 d R U P . .
C11 C 1.0000 0.5062(4) 0.1530(3) 0.2137(19) Uani 1 2 d DS TU P . .
H11A H 0.9083 0.5215 0.1398 0.256 Uiso 0.5 1 d R U P . .
H11B H 1.0917 0.5215 0.1398 0.256 Uiso 0.5 1 d R U P . .
Br1 Br 0.5000 0.18321(5) 0.18253(6) 0.1691(8) Uani 1 2 d S TU P . .
Pb1 Pb 0.5000 0.29874(2) 0.18580(2) 0.07562(11) Uani 1 2 d S TU P . .
Pb3 Pb 0.5000 0.5000 0.0000 0.08439(16) Uani 1 4 d S TU P . .
Pb2 Pb 0.5000 0.39311(2) 0.08772(2) 0.08288(12) Uani 1 2 d S TU P . .
Br3 Br 0.25267(11) 0.31278(4) 0.11817(3) 0.1154(3) Uani 1 1 d . U . . .
Br6 Br 0.5000 0.37497(5) -0.00626(4) 0.1375(5) Uani 1 2 d S TU P . .
Br2 Br 0.2500 0.29824(7) 0.2500 0.1516(6) Uani 1 2 d S TU P . .
Br4 Br 0.5000 0.43197(5) 0.16936(4) 0.1208(5) Uani 1 2 d S TU P . .
Br5 Br 0.24946(12) 0.47853(4) 0.06269(3) 0.1302(3) Uani 1 1 d . U . . .
C13 C 0.0000 0.3817(4) 0.9467(3) 0.2083(19) Uani 1 2 d DS TU P . .
H13A H 0.0923 0.3973 0.9339 0.250 Uiso 0.5 1 d R U P . .
H13B H -0.0923 0.3973 0.9339 0.250 Uiso 0.5 1 d R U P . .
C17 C 0.0000 0.2793(4) 0.9716(3) 0.2109(19) Uani 1 2 d DS TU P . .
H17A H -0.0924 0.2561 0.9689 0.253 Uiso 0.375 1 d R U P . .
H17B H 0.0924 0.2561 0.9689 0.253 Uiso 0.375 1 d R U P . .
C7 C 1.0000 0.4895(4) 0.2265(2) 0.2193(19) Uani 1 2 d DS TU P . .
H7A H 0.9081 0.4974 0.2426 0.263 Uiso 0.375 1 d R U P . .
H7B H 1.0920 0.4974 0.2426 0.263 Uiso 0.375 1 d R U P . .
C12 C 1.0000 0.5296(4) 0.1925(3) 0.220(2) Uani 1 2 d DS TU P . .
H12A H 0.9078 0.5528 0.1953 0.264 Uiso 0.375 1 d R U P . .
H12B H 1.0922 0.5528 0.1953 0.264 Uiso 0.375 1 d R U P . .
C18 C 0.0000 0.3217(4) 0.9384(2) 0.2111(19) Uani 1 2 d DS TU P . .
H18A H 0.0919 0.3141 0.9221 0.253 Uiso 0.375 1 d R U P . .
H18B H -0.0919 0.3141 0.9221 0.253 Uiso 0.375 1 d R U P . .
C8 C 1.0000 0.4290(4) 0.2191(3) 0.2158(19) Uani 1 2 d DS TU P . .
H8A H 1.0923 0.4134 0.2319 0.259 Uiso 0.5 1 d R U P . .
H8B H 0.9077 0.4134 0.2319 0.259 Uiso 0.5 1 d R U P . .
F2 F 0.8542(11) 0.5162(6) 0.2174(4) 0.225(2) Uani 0.5 1 d D U P . .
F1 F 0.6772(19) 0.6006(6) 0.1394(5) 0.208(2) Uani 0.5 1 d . U P . .
F3 F 0.1747(19) 0.2948(6) 0.9560(5) 0.218(2) Uani 0.5 1 d . U P . .
C1 C 0.5000 0.6199(4) 0.1255(3) 0.2018(19) Uani 1 2 d DS TU P . .
H1A H 0.4080 0.6080 0.1107 0.242 Uiso 0.375 1 d R U P . .
H1B H 0.5920 0.6080 0.1107 0.242 Uiso 0.375 1 d R U P . .
C5 C 0.5000 0.6206(4) 0.2011(3) 0.1994(19) Uani 1 2 d DS TU P . .
H5A H 0.4078 0.6093 0.2161 0.239 Uiso 0.5 1 d R U P . .
H5B H 0.5922 0.6093 0.2161 0.239 Uiso 0.5 1 d R U P . .
C2 C 0.5000 0.6790(4) 0.1250(3) 0.1952(19) Uani 1 2 d DS TU P . .
H2A H 0.5918 0.6904 0.1099 0.234 Uiso 0.5 1 d R U P . .
H2B H 0.4082 0.6904 0.1099 0.234 Uiso 0.5 1 d R U P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C3 C4 1.451(12) . ?
C3 C2 1.460(12) . ?
C4 C5 1.452(11) . ?
C10 C9 1.413(12) . ?
C10 C11 1.473(12) . ?
C9 C8 1.439(12) . ?
C14 C15 1.414(12) . ?
C14 C13 1.437(12) . ?
C15 C16 1.411(12) . ?
C16 C17 1.478(12) . ?
C6 C5 1.447(12) . ?
C6 C1 1.467(12) . ?
C6 F1 1.713(17) . ?
C6 F1 1.713(17) 12_655 ?
C11 C12 1.437(12) . ?
Br1 Pb1 2.7908(14) . ?
Pb1 Br2 2.9983(3) 14_556 ?
Pb1 Br2 2.9983(3) . ?
Pb1 Br3 3.0846(9) . ?
Pb1 Br3 3.0846(10) 12_655 ?
Pb3 Br5 3.0104(10) 12_655 ?
Pb3 Br5 3.0104(10) 4_565 ?
Pb3 Br5 3.0104(10) 9_665 ?
Pb3 Br5 3.0105(10) . ?
Pb3 Br6 3.0250(13) 9_665 ?
Pb3 Br6 3.0251(13) . ?
Pb2 Br4 2.8833(13) . ?
Pb2 Br3 3.0154(9) 12_655 ?
Pb2 Br3 3.0154(9) . ?
Pb2 Br5 3.0597(10) . ?
Pb2 Br5 3.0597(11) 12_655 ?
Pb2 Br6 3.1691(14) . ?
Br2 Pb1 2.9983(3) 14_456 ?
C13 C18 1.474(12) . ?
C17 C18 1.508(12) . ?
C17 F3 1.599(17) 12 ?
C17 F3 1.599(17) . ?
C7 F2 1.415(11) . ?
C7 F2 1.415(11) 12_755 ?
C7 C8 1.483(12) . ?
C7 C12 1.489(12) . ?
C12 F2 1.512(11) 12_755 ?
C12 F2 1.512(11) . ?
C18 F3 1.707(17) . ?
C18 F3 1.707(17) 12 ?
F1 C1 1.625(16) . ?
C1 C2 1.427(12) . ?
C1 F1 1.625(16) 12_655 ?

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
C4 C3 C2 121.2(8) . . ?
C3 C4 C5 118.9(8) . . ?
C9 C10 C11 118.5(9) . . ?
C10 C9 C8 122.5(9) . . ?
C15 C14 C13 124.5(9) . . ?
C16 C15 C14 118.4(9) . . ?
C15 C16 C17 124.2(9) . . ?
C5 C6 C1 120.2(8) . . ?
C5 C6 F1 109.6(6) . . ?
C1 C6 F1 60.9(6) . . ?
C5 C6 F1 109.6(6) . 12_655 ?
C1 C6 F1 60.9(6) . 12_655 ?
F1 C6 F1 120.3(12) . 12_655 ?
C12 C11 C10 123.2(9) . . ?
Br1 Pb1 Br2 91.37(4) . 14_556 ?
Br1 Pb1 Br2 91.38(4) . . ?
Br2 Pb1 Br2 88.692(11) 14_556 . ?
Br1 Pb1 Br3 94.65(3) . . ?
Br2 Pb1 Br3 173.66(4) 14_556 . ?
Br2 Pb1 Br3 93.107(19) . . ?
Br1 Pb1 Br3 94.66(3) . 12_655 ?
Br2 Pb1 Br3 93.108(19) 14_556 12_655 ?
Br2 Pb1 Br3 173.66(4) . 12_655 ?
Br3 Pb1 Br3 84.47(4) . 12_655 ?
Br5 Pb3 Br5 180.0 12_655 4_565 ?
Br5 Pb3 Br5 91.52(4) 12_655 9_665 ?
Br5 Pb3 Br5 88.48(4) 4_565 9_665 ?
Br5 Pb3 Br5 88.48(4) 12_655 . ?
Br5 Pb3 Br5 91.52(4) 4_565 . ?
Br5 Pb3 Br5 180.0 9_665 . ?
Br5 Pb3 Br6 97.11(3) 12_655 9_665 ?
Br5 Pb3 Br6 82.89(3) 4_565 9_665 ?
Br5 Pb3 Br6 82.89(3) 9_665 9_665 ?
Br5 Pb3 Br6 97.10(3) . 9_665 ?
Br5 Pb3 Br6 82.89(3) 12_655 . ?
Br5 Pb3 Br6 97.11(3) 4_565 . ?
Br5 Pb3 Br6 97.11(3) 9_665 . ?
Br5 Pb3 Br6 82.90(3) . . ?
Br6 Pb3 Br6 180.0 9_665 . ?
Br4 Pb2 Br3 83.70(3) . 12_655 ?
Br4 Pb2 Br3 83.70(3) . . ?
Br3 Pb2 Br3 86.88(4) 12_655 . ?
Br4 Pb2 Br5 92.24(3) . . ?
Br3 Pb2 Br5 175.93(3) 12_655 . ?
Br3 Pb2 Br5 93.07(3) . . ?
Br4 Pb2 Br5 92.25(3) . 12_655 ?
Br3 Pb2 Br5 93.07(3) 12_655 12_655 ?
Br3 Pb2 Br5 175.93(3) . 12_655 ?
Br5 Pb2 Br5 86.70(4) . 12_655 ?
Br4 Pb2 Br6 168.95(4) . . ?
Br3 Pb2 Br6 104.19(3) 12_655 . ?
Br3 Pb2 Br6 104.19(3) . . ?
Br5 Pb2 Br6 79.77(3) . . ?
Br5 Pb2 Br6 79.77(3) 12_655 . ?
Pb2 Br3 Pb1 81.69(2) . . ?
Pb3 Br6 Pb2 78.10(3) . . ?
Pb1 Br2 Pb1 179.54(6) . 14_456 ?
Pb3 Br5 Pb2 80.05(2) . . ?
C14 C13 C18 116.6(8) . . ?
C16 C17 C18 114.4(8) . . ?
C16 C17 F3 102.0(7) . 12 ?
C18 C17 F3 66.6(7) . 12 ?
C16 C17 F3 102.0(7) . . ?
C18 C17 F3 66.6(7) . . ?
F3 C17 F3 132.8(14) 12 . ?
F2 C7 F2 119.6(12) . 12_755 ?
F2 C7 C8 114.4(7) . . ?
F2 C7 C8 114.4(7) 12_755 . ?
F2 C7 C12 62.7(6) . . ?
F2 C7 C12 62.7(6) 12_755 . ?
C8 C7 C12 120.9(8) . . ?
C11 C12 C7 116.4(8) . . ?
C11 C12 F2 114.9(7) . 12_755 ?
C7 C12 F2 56.2(6) . 12_755 ?
C11 C12 F2 114.9(7) . . ?
C7 C12 F2 56.2(6) . . ?
F2 C12 F2 107.9(11) 12_755 . ?
C13 C18 C17 121.9(8) . . ?
C13 C18 F3 108.0(6) . . ?
C17 C18 F3 59.3(6) . . ?
C13 C18 F3 108.0(6) . 12 ?
C17 C18 F3 59.2(6) . 12 ?
F3 C18 F3 118.2(12) . 12 ?
C9 C8 C7 118.4(8) . . ?
C7 F2 C12 61.1(6) . . ?
C1 F1 C6 52.1(6) . . ?
C17 F3 C18 54.2(7) . . ?
C2 C1 C6 119.9(9) . . ?
C2 C1 F1 106.8(7) . 12_655 ?
C6 C1 F1 67.1(7) . 12_655 ?
C2 C1 F1 106.8(7) . . ?
C6 C1 F1 67.1(7) . . ?
F1 C1 F1 132.2(13) 12_655 . ?
C6 C5 C4 120.2(9) . . ?
C1 C2 C3 119.6(9) . . ?

_refine_diff_density_max         0.533
_refine_diff_density_min         -0.806
_refine_diff_density_rms         0.133



_vrf_PLAT241_cmca                
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of        Br6 Check 
RESPONSE: The alert is due to the highly disordered molecule.
;
_vrf_PLAT242_cmca                
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        Pb1 Check 
RESPONSE: The alert is due to the highly disordered molecule.
;

####################################################################### 
# 
# 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_hxq_220503_1_323kk_auto
_database_code_depnum_ccdc_archive 'CCDC 2195160'
loop_
_audit_author_name
_audit_author_address
'Zhong-Xia Wang'
;Nanchang University
China
;
_audit_update_record             
;
2022-08-05 deposited with the CCDC.	2023-12-03 downloaded from the CCDC.
;
_audit_creation_date             2022-05-17
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br3 Pb, C5 H12 N'
_chemical_formula_sum            'C5 H12 Br3 N Pb'
_chemical_formula_weight         533.08
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C N H Pb  Br'
_chemical_oxdiff_usercomment     \
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   9.8560(5)
_cell_length_b                   7.8629(4)
_cell_length_c                   15.1092(7)
_cell_angle_alpha                90
_cell_angle_beta                 102.382(5)
_cell_angle_gamma                90
_cell_volume                     1143.68(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3969
_cell_measurement_temperature    323.02(11)
_cell_measurement_theta_max      29.2330
_cell_measurement_theta_min      2.2650
_shelx_estimated_absorpt_T_max   0.633
_shelx_estimated_absorpt_T_min   0.432
_exptl_absorpt_coefficient_mu    25.177
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.07773
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.108a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.096
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       strip
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0690
_diffrn_reflns_av_unetI/netI     0.0538
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.782
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9854
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.782
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.888
_diffrn_reflns_theta_min         2.265
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      323.02(11)
_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 0.782
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -14.00  28.00   0.50    1.00    --   -5.27 -99.00 -30.00   84
  2  ω     -3.00  26.00   0.50    1.00    --   -5.27 -99.00-180.00   58
  3  ω    -78.00  -8.00   0.50    1.00    --   -5.27 -54.00 -61.00  140
  4  ω    -16.00  67.00   0.50    1.00    --   -5.27  54.00  82.00  166
  5  ω     -7.00  26.00   0.50    1.00    --    5.11  37.00 150.00   66
;
_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      0.0500723000
_diffrn_orient_matrix_UB_12      -0.0593230000
_diffrn_orient_matrix_UB_13      0.0222568000
_diffrn_orient_matrix_UB_21      0.0234794000
_diffrn_orient_matrix_UB_22      -0.0120937000
_diffrn_orient_matrix_UB_23      -0.0407637000
_diffrn_orient_matrix_UB_31      0.0486859000
_diffrn_orient_matrix_UB_32      0.0668804000
_diffrn_orient_matrix_UB_33      0.0123489000
_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                1982
_reflns_number_total             2826
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_refine_diff_density_max         3.300
_refine_diff_density_min         -2.612
_refine_diff_density_rms         0.339
_refine_ls_extinction_coef       0.0048(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         2826
_refine_ls_number_restraints     276
_refine_ls_R_factor_all          0.0860
_refine_ls_R_factor_gt           0.0593
_refine_ls_restrained_S_all      1.003
_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)+(0.1059P)²+5.7582P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1690
_refine_ls_wR_factor_ref         0.1853
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.01 and sigma
for terminal atoms of 0.02
3. Others
 Fixed Sof: N1(0.5) H1A(0.5) H1B(0.5) C1(0.5) H1C(0.5) H1D(0.5) C3(0.5)
 H3A(0.5) H3B(0.5) C4(0.5) H4A(0.5) H4B(0.5) C2(0.5) H2A(0.5) H2B(0.5) C5(0.5)
 H5A(0.5) H5B(0.5) N1'(0.5) H1'A(0.5) H1'B(0.5) C1'(0.5) H1'C(0.5) H1'D(0.5)
 C3'(0.5) H3'A(0.5) H3'B(0.5) C4'(0.5) H4'A(0.5) H4'B(0.5) C2'(0.5) H2'A(0.5)
 H2'B(0.5) C5'(0.5) H5'A(0.5) H5'B(0.5)
4.a Riding coordinates:
 N1(H1A,H1B), C1(H1C,H1D), C3(H3A,H3B), C4(H4A,H4B), C2(H2A,H2B), C5(H5A,H5B),
 N1'(H1'A,H1'B), C1'(H1'C,H1'D), C3'(H3'A,H3'B), C4'(H4'A,H4'B), C2'(H2'A,H2'B),
  C5'(H5'A,H5'B)
;
_atom_sites_solution_hydrogens   difmap
_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 0.74960(4) 0.00461(5) 0.74649(3) 0.0437(3) Uani 1 1 d . U . . .
Br1 Br 0.55660(16) 0.23663(15) 0.81552(11) 0.0569(4) Uani 1 1 d . U . . .
Br2 Br 0.79146(17) -0.20646(19) 0.90648(8) 0.0599(4) Uani 1 1 d . U . . .
Br3 Br 0.96643(15) 0.22768(19) 0.84470(11) 0.0630(4) Uani 1 1 d . U . . .
N1 N 0.342(3) 0.333(4) 0.5695(19) 0.068(4) Uani 0.5 1 d . U P A 1
H1A H 0.372300 0.381993 0.523467 0.082 Uiso 0.5 1 d R U P A 1
H1B H 0.409120 0.344013 0.620077 0.082 Uiso 0.5 1 d R U P A 1
C1 C 0.347(4) 0.146(5) 0.564(3) 0.067(4) Uani 0.5 1 d . U P A 1
H1C H 0.397153 0.154390 0.626026 0.081 Uiso 0.5 1 d R U P A 1
H1D H 0.402733 0.084520 0.530056 0.081 Uiso 0.5 1 d R U P A 1
C3 C 0.144(4) 0.146(4) 0.645(2) 0.066(4) Uani 0.5 1 d . U P A 1
H3A H 0.064345 0.092464 0.660085 0.079 Uiso 0.5 1 d R U P A 1
H3B H 0.217015 0.154454 0.697785 0.079 Uiso 0.5 1 d R U P A 1
C4 C 0.106(4) 0.331(4) 0.600(2) 0.068(4) Uani 0.5 1 d . U P A 1
H4A H 0.049958 0.396611 0.631895 0.082 Uiso 0.5 1 d R U P A 1
H4B H 0.058838 0.320451 0.537335 0.082 Uiso 0.5 1 d R U P A 1
C2 C 0.237(4) 0.043(4) 0.606(2) 0.068(4) Uani 0.5 1 d . U P A 1
H2A H 0.294456 0.041433 0.666156 0.081 Uiso 0.5 1 d R U P A 1
H2B H 0.212766 -0.072167 0.588836 0.081 Uiso 0.5 1 d R U P A 1
C5 C 0.261(4) 0.410(5) 0.609(2) 0.069(4) Uani 0.5 1 d . U P A 1
H5A H 0.259059 0.530961 0.599669 0.082 Uiso 0.5 1 d R U P A 1
H5B H 0.318889 0.384481 0.667319 0.082 Uiso 0.5 1 d R U P A 1
N1' N 0.312(3) 0.306(4) 0.5311(17) 0.066(3) Uani 0.5 1 d . U P B 2
H1'A H 0.242642 0.299488 0.481524 0.079 Uiso 0.5 1 d R U P B 2
H1'B H 0.385722 0.356868 0.516124 0.079 Uiso 0.5 1 d R U P B 2
C1' C 0.310(4) 0.113(5) 0.548(3) 0.067(4) Uani 0.5 1 d . U P B 2
H1'C H 0.396745 0.053444 0.554388 0.081 Uiso 0.5 1 d R U P B 2
H1'D H 0.259115 0.099804 0.486978 0.081 Uiso 0.5 1 d R U P B 2
C3' C 0.102(3) 0.146(4) 0.607(2) 0.066(4) Uani 0.5 1 d . U P B 2
H3'A H 0.050280 0.093172 0.646757 0.080 Uiso 0.5 1 d R U P B 2
H3'B H 0.043410 0.150982 0.547157 0.080 Uiso 0.5 1 d R U P B 2
C4' C 0.150(4) 0.332(4) 0.642(2) 0.068(4) Uani 0.5 1 d . U P B 2
H4'A H 0.211591 0.324473 0.700231 0.082 Uiso 0.5 1 d R U P B 2
H4'B H 0.070791 0.397653 0.647751 0.082 Uiso 0.5 1 d R U P B 2
C2' C 0.196(4) 0.046(4) 0.564(2) 0.066(4) Uani 0.5 1 d . U P B 2
H2'A H 0.206778 -0.074146 0.575100 0.079 Uiso 0.5 1 d R U P B 2
H2'B H 0.134218 0.065424 0.506890 0.079 Uiso 0.5 1 d R U P B 2
C5' C 0.217(4) 0.416(5) 0.581(2) 0.069(4) Uani 0.5 1 d . U P B 2
H5'A H 0.154275 0.425442 0.522908 0.083 Uiso 0.5 1 d R U P B 2
H5'B H 0.240395 0.529782 0.602398 0.083 Uiso 0.5 1 d R U P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br1 3.1199(14) 2_646 ?
Pb1 Br1 2.9808(14) . ?
Pb1 Br2 2.8879(13) . ?
Pb1 Br2 3.2039(14) 2_656 ?
Pb1 Br3 3.1488(15) 2_646 ?
Pb1 Br3 2.9129(15) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
N1 C1 1.47(5) . ?
N1 C5 1.26(4) . ?
C1 H1C 0.9600 . ?
C1 H1D 0.9600 . ?
C1 C2 1.59(5) . ?
C3 H3A 0.9599 . ?
C3 H3B 0.9600 . ?
C3 C4 1.61(4) . ?
C3 C2 1.44(5) . ?
C4 H4A 0.9601 . ?
C4 H4B 0.9599 . ?
C4 C5 1.63(5) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C5 H5A 0.9599 . ?
C5 H5B 0.9600 . ?
N1' H1'A 0.9000 . ?
N1' H1'B 0.9000 . ?
N1' C1' 1.54(5) . ?
N1' C5' 1.58(5) . ?
C1' H1'C 0.9600 . ?
C1' H1'D 0.9600 . ?
C1' C2' 1.31(5) . ?
C3' H3'A 0.9600 . ?
C3' H3'B 0.9600 . ?
C3' C4' 1.59(5) . ?
C3' C2' 1.47(5) . ?
C4' H4'A 0.9600 . ?
C4' H4'B 0.9600 . ?
C4' C5' 1.41(5) . ?
C2' H2'A 0.9599 . ?
C2' H2'B 0.9601 . ?
C5' H5'A 0.9599 . ?
C5' H5'B 0.9599 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br1 Pb1 Br1 174.97(4) . 2_646 ?
Br1 Pb1 Br2 104.66(4) 2_646 2_656 ?
Br1 Pb1 Br2 80.04(4) . 2_656 ?
Br1 Pb1 Br3 78.56(4) 2_646 2_646 ?
Br1 Pb1 Br3 98.86(4) . 2_646 ?
Br2 Pb1 Br1 92.65(4) . . ?
Br2 Pb1 Br1 82.90(4) . 2_646 ?
Br2 Pb1 Br2 169.92(5) . 2_656 ?
Br2 Pb1 Br3 86.02(4) . 2_646 ?
Br2 Pb1 Br3 87.83(5) . . ?
Br3 Pb1 Br1 97.48(4) . 2_646 ?
Br3 Pb1 Br1 84.65(5) . . ?
Br3 Pb1 Br2 84.60(4) . 2_656 ?
Br3 Pb1 Br2 101.87(4) 2_646 2_656 ?
Br3 Pb1 Br3 173.05(4) . 2_646 ?
Pb1 Br1 Pb1 80.24(4) . 2_656 ?
Pb1 Br2 Pb1 80.24(3) . 2_646 ?
Pb1 Br3 Pb1 80.80(3) . 2_656 ?
H1A N1 H1B 108.1 . . ?
C1 N1 H1A 111.6 . . ?
C1 N1 H1B 96.8 . . ?
C5 N1 H1A 120.6 . . ?
C5 N1 H1B 88.4 . . ?
C5 N1 C1 123(3) . . ?
N1 C1 H1C 83.8 . . ?
N1 C1 H1D 123.9 . . ?
N1 C1 C2 117(3) . . ?
H1C C1 H1D 108.9 . . ?
C2 C1 H1C 84.4 . . ?
C2 C1 H1D 118.6 . . ?
H3A C3 H3B 109.5 . . ?
C4 C3 H3A 111.9 . . ?
C4 C3 H3B 111.1 . . ?
C2 C3 H3A 118.2 . . ?
C2 C3 H3B 86.6 . . ?
C2 C3 C4 117(3) . . ?
C3 C4 H4A 112.3 . . ?
C3 C4 H4B 111.1 . . ?
C3 C4 C5 100(2) . . ?
H4A C4 H4B 109.6 . . ?
C5 C4 H4A 112.0 . . ?
C5 C4 H4B 111.2 . . ?
C1 C2 H2A 94.0 . . ?
C1 C2 H2B 121.6 . . ?
C3 C2 C1 115(3) . . ?
C3 C2 H2A 85.6 . . ?
C3 C2 H2B 119.8 . . ?
H2A C2 H2B 107.8 . . ?
N1 C5 H1B 36.2 . . ?
N1 C5 C4 117(3) . . ?
N1 C5 H5A 113.7 . . ?
N1 C5 H5B 91.2 . . ?
H1B C5 H5A 110.0 . . ?
H1B C5 H5B 57.5 . . ?
C4 C5 H1B 137.5 . . ?
C4 C5 H5A 112.2 . . ?
C4 C5 H5B 111.2 . . ?
H5A C5 H5B 109.6 . . ?
H1'A N1' H1'B 109.1 . . ?
C1' N1' H1'A 92.9 . . ?
C1' N1' H1'B 121.2 . . ?
C1' N1' C5' 116(3) . . ?
C5' N1' H1'A 90.4 . . ?
C5' N1' H1'B 117.9 . . ?
N1' C1' H1'C 117.2 . . ?
N1' C1' H1'D 88.1 . . ?
H1'C C1' H1'D 108.2 . . ?
C2' C1' N1' 118(3) . . ?
C2' C1' H1'C 124.3 . . ?
C2' C1' H1'D 80.8 . . ?
H3'A C3' H3'B 108.6 . . ?
C4' C3' H3'A 110.6 . . ?
C4' C3' H3'B 110.4 . . ?
C2' C3' H3'A 120.9 . . ?
C2' C3' H3'B 85.3 . . ?
C2' C3' C4' 117(3) . . ?
C3' C4' H4'A 109.4 . . ?
C3' C4' H4'B 109.2 . . ?
H4'A C4' H4'B 108.0 . . ?
C5' C4' C3' 112(3) . . ?
C5' C4' H4'A 110.0 . . ?
C5' C4' H4'B 108.4 . . ?
C1' C2' H1'D 39.4 . . ?
C1' C2' C3' 121(3) . . ?
C1' C2' H2'A 111.4 . . ?
C1' C2' H2'B 100.2 . . ?
H1'D C2' H2'A 111.5 . . ?
H1'D C2' H2'B 62.7 . . ?
C3' C2' H1'D 126.7 . . ?
C3' C2' H2'A 120.3 . . ?
C3' C2' H2'B 88.1 . . ?
H2'A C2' H2'B 109.6 . . ?
N1' C5' H5'A 86.5 . . ?
N1' C5' H5'B 123.4 . . ?
C4' C5' N1' 117(3) . . ?
C4' C5' H5'A 109.2 . . ?
C4' C5' H5'B 109.0 . . ?
H5'A C5' H5'B 107.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 0(4) . . . . ?
C1 N1 C5 C4 -38(4) . . . . ?
C3 C4 C5 N1 61(4) . . . . ?
C4 C3 C2 C1 30(4) . . . . ?
C2 C3 C4 C5 -56(3) . . . . ?
C5 N1 C1 C2 4(4) . . . . ?
N1' C1' C2' C3' -29(5) . . . . ?
C1' N1' C5' C4' 5(4) . . . . ?
C3' C4' C5' N1' -37(4) . . . . ?
C4' C3' C2' C1' -6(5) . . . . ?
C2' C3' C4' C5' 40(4) . . . . ?
C5' N1' C1' C2' 30(4) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 5.687
_oxdiff_exptl_absorpt_empirical_full_min 0.341
####################################################################### 
# 
# 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_hxq_211027_2_auto
_database_code_depnum_ccdc_archive 'CCDC 2195164'
loop_
_audit_author_name
_audit_author_address
'Zhong-Xia Wang'
;Nanchang University
China
;
_audit_update_record             
;
2022-08-05 deposited with the CCDC.	2023-12-03 downloaded from the CCDC.
;
_audit_creation_date             2022-01-18
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br12 Pb3, 6(C5 H10 F2 N)'
_chemical_formula_sum            'C30 H60 Br12 F12 N6 Pb3'
_chemical_formula_weight         2313.33
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H N F Pb Br'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.1732(3)
_cell_length_b                   13.4785(4)
_cell_length_c                   18.4607(5)
_cell_angle_alpha                76.808(2)
_cell_angle_beta                 89.923(2)
_cell_angle_gamma                76.288(2)
_cell_volume                     2860.53(14)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    19351
_cell_measurement_temperature    289.99(10)
_cell_measurement_theta_max      30.9130
_cell_measurement_theta_min      2.1960
_shelx_estimated_absorpt_T_max   0.724
_shelx_estimated_absorpt_T_min   0.545
_exptl_absorpt_coefficient_mu    17.257
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.12050
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.108a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.686
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0876
_diffrn_reflns_av_unetI/netI     0.0779
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.806
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            47501
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.806
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.954
_diffrn_reflns_theta_min         1.725
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      289.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.806
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -19.00   7.00   0.50    1.00    --    5.05  85.00  15.00   52
  2  ω     30.00  78.00   0.50    1.00    --    5.05  37.00  60.00   96
  3  ω      9.00  36.00   0.50    1.00    --    5.05 -99.00  30.00   54
  4  ω    -30.00  28.00   0.50    1.00    --    5.05 -85.00-103.00  116
  5  ω    -18.00  68.00   0.50    1.00    --   -5.21  37.00 -30.00  172
  6  ω    -32.00  41.00   0.50    1.00    --   -5.21  85.00  15.00  146
  7  ω    -18.00  28.00   0.50    1.00    --   -5.21 -99.00  60.00   92
  8  ω    -16.00  27.00   0.50    1.00    --   -5.21 -99.00-150.00   86
  9  ω    -10.00  18.00   0.50    1.00    --   -5.21 -77.00-150.00   56
 10  ω    -73.00 -17.00   0.50    1.00    --   -5.21 -77.00-150.00  112
;
_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      0.0306773000
_diffrn_orient_matrix_UB_12      -0.0265017000
_diffrn_orient_matrix_UB_13      -0.0255690000
_diffrn_orient_matrix_UB_21      0.0494372000
_diffrn_orient_matrix_UB_22      -0.0141981000
_diffrn_orient_matrix_UB_23      0.0240402000
_diffrn_orient_matrix_UB_31      -0.0149425000
_diffrn_orient_matrix_UB_32      -0.0469164000
_diffrn_orient_matrix_UB_33      0.0181804000
_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                10124
_reflns_number_total             14640
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         9.386
_refine_diff_density_min         -4.152
_refine_diff_density_rms         0.570
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     571
_refine_ls_number_reflns         14640
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1229
_refine_ls_R_factor_gt           0.0848
_refine_ls_restrained_S_all      1.020
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1569P)²+27.4751P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2257
_refine_ls_wR_factor_ref         0.2510
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
2. Uiso/Uaniso restraints and constraints
F00Y \\sim F00J \\sim F00Q \\sim F00K \\sim F00P \\sim F00M \\sim F00T \\sim
F00I \\sim F00N \\sim F00H \\sim F1 \\sim F00O: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.01 within 2A
Uanis(F00P) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
3. Rigid body (RIGU) restrains
 F00O, F1, F00M, F00P, F00T, F00I, F00H, F00N, F00J, F00Y, F00Q, F00K
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4.a Secondary CH2 refined with riding coordinates:
 C00U(H00c,H00d), C00V(H00g,H00h), N00X(H00e,H00f), C00Z(H00a,H00b), C011(H01a,
 H01b), C012(H01,H), N013(H01k,H01l), C015(H01u,H01v), N016(H01c,H01d),
 C017(H01q,H01r), N018(H1,Ha), C01A(H01m,H01n), C01B(H5,Hb), N01C(H6,Hc),
 C01D(H01e,H01f), C01E(H01g,H01h), C01F(H2,Hd), N01G(H01w,H01x), C01H(H7,He),
 C01I(H01y,Hf), C01J(H01s,H01t), C01K(H01o,H01p), C01L(H3,Hg), C01M(H01i,H01j),
 C01N(H8,Hh), C01O(H4,Hi), C01P(H01z,Hj), C21(H21a,H21b), C23(H23a,H23b),
 C26(H26a,H26b)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb01 Pb 0.24900(3) 1.00453(3) 0.51654(2) 0.02377(9) Uani 1 1 d . . . . .
Pb02 Pb 0.25166(3) 0.98580(3) 0.19005(2) 0.02334(9) Uani 1 1 d . . . . .
Pb03 Pb 0.24750(3) 1.01321(3) 0.85067(2) 0.02465(9) Uani 1 1 d . . . . .
Br04 Br 0.48697(9) 0.99136(9) 0.16782(7) 0.0380(3) Uani 1 1 d . . . . .
Br05 Br 0.19881(10) 1.21733(9) 0.15412(7) 0.0384(3) Uani 1 1 d . . . . .
Br06 Br 0.29805(10) 0.77585(9) 0.56351(7) 0.0375(3) Uani 1 1 d . . . . .
Br07 Br 0.33095(9) 0.75524(9) 0.26049(7) 0.0372(3) Uani 1 1 d . . . . .
Br08 Br 0.17193(9) 1.24266(10) 0.84711(7) 0.0391(3) Uani 1 1 d . . . . .
Br09 Br 0.34418(10) 0.78045(10) 0.88731(6) 0.0383(3) Uani 1 1 d . . . . .
Br0A Br 0.14880(10) 1.23902(10) 0.47714(6) 0.0385(3) Uani 1 1 d . . . . .
Br0B Br 0.000000 1.000000 0.500000 0.0449(5) Uani 1 2 d S . P . .
Br0C Br 0.01239(9) 1.00831(9) 0.83216(7) 0.0390(3) Uani 1 1 d . . . . .
Br0D Br 0.26781(11) 1.00902(11) 0.67879(6) 0.0446(3) Uani 1 1 d . . . . .
Br0E Br 0.22599(12) 0.99379(11) 1.01475(6) 0.0467(4) Uani 1 1 d . . . . .
Br0F Br 0.25245(12) 1.00006(11) 0.34875(6) 0.0480(4) Uani 1 1 d . . . . .
Br0G Br 0.500000 1.000000 0.500000 0.0512(5) Uani 1 2 d S . P . .
F00H F -0.1011(8) 0.3855(7) 0.6977(4) 0.066(3) Uani 1 1 d . . . . .
F00I F 0.2247(7) 0.6037(8) 0.7365(6) 0.077(3) Uani 1 1 d . . . . .
F00J F 0.7222(7) 0.5998(8) 0.7304(6) 0.079(3) Uani 1 1 d . . . . .
F00K F 0.2711(8) 0.4213(8) 0.5531(5) 0.077(3) Uani 1 1 d . . . . .
F1 F 0.2301(7) 0.5800(7) 1.0251(5) 0.073(3) Uani 1 1 d . . . . .
F00M F 0.3982(8) 0.3883(8) 0.8452(5) 0.073(3) Uani 1 1 d . . . . .
F00N F 0.0557(7) 0.4197(7) 0.6538(6) 0.077(3) Uani 1 1 d . . . . .
F00O F 0.1152(10) 0.4887(6) 1.0782(6) 0.095(4) Uani 1 1 d . . . . .
F00P F 0.5549(8) 0.4169(8) 0.8760(6) 0.087(3) Uani 1 1 d . U . . .
F00Q F 0.3846(11) 0.5108(7) 0.5772(7) 0.115(4) Uani 1 1 d . . . . .
C00R C 0.3717(12) 0.4120(10) 0.5903(8) 0.051(4) Uani 1 1 d . . . . .
C00S C 0.6382(10) 0.6274(10) 0.6749(7) 0.041(3) Uani 1 1 d . . . . .
F00T F 0.1964(8) 0.5862(9) 0.8528(5) 0.091(4) Uani 1 1 d . . . . .
C00U C 0.5429(10) 0.5792(10) 0.7056(7) 0.043(3) Uani 1 1 d . . . . .
H00C H 0.488769 0.585133 0.665380 0.052 Uiso 1 1 calc R U . . .
H00D H 0.572681 0.505228 0.728485 0.052 Uiso 1 1 calc R U . . .
C00V C 0.4193(12) 0.4081(12) 0.9657(8) 0.059(4) Uani 1 1 d . . . . .
H00G H 0.477036 0.408799 1.001570 0.070 Uiso 1 1 calc R U . . .
H00H H 0.376990 0.479946 0.945676 0.070 Uiso 1 1 calc R U . . .
C00W C 0.1273(12) 0.5897(11) 1.0596(7) 0.049(4) Uani 1 1 d . . . . .
N00X N 0.4468(7) 0.7505(8) 0.7267(5) 0.038(3) Uani 1 1 d . . . . .
H00E H 0.398092 0.760664 0.688281 0.046 Uiso 1 1 calc R U . . .
H00F H 0.411298 0.783750 0.759741 0.046 Uiso 1 1 calc R U . . .
F00Y F 0.6861(9) 0.5743(10) 0.6219(6) 0.099(4) Uani 1 1 d . . . . .
C00Z C -0.0140(12) 0.6316(11) 0.7010(9) 0.055(4) Uani 1 1 d . . . . .
H00A H -0.077967 0.601808 0.696131 0.066 Uiso 1 1 calc R U . . .
H00B H 0.036007 0.618621 0.661406 0.066 Uiso 1 1 calc R U . . .
C010 C 0.1437(11) 0.6319(11) 0.7842(7) 0.047(4) Uani 1 1 d . . . . .
C011 C -0.0833(11) 0.4111(10) 0.5688(7) 0.047(4) Uani 1 1 d . . . . .
H01A H -0.026869 0.411230 0.531679 0.056 Uiso 1 1 calc R U . . .
H01B H -0.125966 0.482975 0.564561 0.056 Uiso 1 1 calc R U . . .
C012 C 0.1394(12) 0.6274(12) 1.1265(8) 0.056(4) Uani 1 1 d . . . . .
H01 H 0.207632 0.584283 1.155276 0.068 Uiso 1 1 calc R U . . .
H H 0.075513 0.619678 1.156878 0.068 Uiso 1 1 calc R U . . .
N013 N -0.0551(8) 0.7482(9) 0.6937(6) 0.048(3) Uani 1 1 d . . . . .
H01K H -0.091685 0.778017 0.649497 0.058 Uiso 1 1 calc R U . . .
H01L H -0.103519 0.759957 0.728760 0.058 Uiso 1 1 calc R U . . .
C014 C -0.0262(10) 0.3670(9) 0.6453(7) 0.039(3) Uani 1 1 d . . . . .
C015 C 0.3609(12) 0.3723(13) 0.6710(8) 0.060(4) Uani 1 1 d . . . . .
H01U H 0.293105 0.414252 0.686914 0.072 Uiso 1 1 calc R U . . .
H01V H 0.425672 0.378138 0.698899 0.072 Uiso 1 1 calc R U . . .
N016 N -0.0997(9) 0.2331(8) 0.5679(6) 0.049(3) Uani 1 1 d . . . . .
H01C H -0.146443 0.195308 0.558372 0.059 Uiso 1 1 calc R U . . .
H01D H -0.045124 0.228275 0.535828 0.059 Uiso 1 1 calc R U . . .
C017 C 0.4854(11) 0.6343(11) 0.7621(7) 0.050(4) Uani 1 1 d . . . . .
H01Q H 0.537371 0.622673 0.804646 0.060 Uiso 1 1 calc R U . . .
H01R H 0.420739 0.606803 0.779234 0.060 Uiso 1 1 calc R U . . .
N018 N 0.0507(8) 0.8073(7) 1.0549(6) 0.038(3) Uani 1 1 d . . . . .
H1 H 0.059706 0.872556 1.042183 0.046 Uiso 1 1 calc R U . . .
HA H -0.014569 0.809351 1.076972 0.046 Uiso 1 1 calc R U . . .
C019 C 0.4746(10) 0.3630(9) 0.9037(6) 0.036(3) Uani 1 1 d . . . . .
C01A C 0.0479(11) 0.5802(11) 0.7748(8) 0.053(4) Uani 1 1 d . . . . .
H01M H 0.078430 0.505950 0.777812 0.064 Uiso 1 1 calc R U . . .
H01N H -0.003865 0.587088 0.814372 0.064 Uiso 1 1 calc R U . . .
C01B C 0.3418(11) 0.3450(11) 1.0034(8) 0.056(4) Uani 1 1 d . . . . .
H5 H 0.276272 0.355264 0.970159 0.067 Uiso 1 1 calc R U . . .
HB H 0.315490 0.368950 1.047503 0.067 Uiso 1 1 calc R U . . .
N01C N 0.4009(8) 0.2293(9) 1.0253(6) 0.050(3) Uani 1 1 d . . . . .
H6 H 0.455912 0.219448 1.059808 0.060 Uiso 1 1 calc R U . . .
HC H 0.351483 0.193207 1.045482 0.060 Uiso 1 1 calc R U . . .
C01D C -0.1629(11) 0.3438(12) 0.5555(8) 0.062(4) Uani 1 1 d . . . . .
H01E H -0.224005 0.349930 0.589259 0.074 Uiso 1 1 calc R U . . .
H01F H -0.195755 0.368591 0.504872 0.074 Uiso 1 1 calc R U . . .
C01E C 0.0307(9) 0.2503(9) 0.6607(7) 0.037(3) Uani 1 1 d . . . . .
H01G H 0.096161 0.239570 0.630814 0.045 Uiso 1 1 calc R U . . .
H01H H 0.056799 0.224956 0.712753 0.045 Uiso 1 1 calc R U . . .
C01F C 0.0345(11) 0.6569(11) 1.0054(7) 0.047(3) Uani 1 1 d . . . . .
H2 H -0.037948 0.654526 1.026779 0.056 Uiso 1 1 calc R U . . .
HD H 0.037071 0.630332 0.960693 0.056 Uiso 1 1 calc R U . . .
N01G N 0.4503(9) 0.1944(8) 0.6551(7) 0.052(3) Uani 1 1 d . . . . .
H01W H 0.514179 0.195194 0.678115 0.062 Uiso 1 1 calc R U . . .
H01X H 0.444703 0.128111 0.664594 0.062 Uiso 1 1 calc R U . . .
C01H C 0.5282(10) 0.2462(9) 0.9229(6) 0.041(3) Uani 1 1 d . . . . .
H7 H 0.547843 0.222774 0.877620 0.049 Uiso 1 1 calc R U . . .
HE H 0.597163 0.231795 0.953804 0.049 Uiso 1 1 calc R U . . .
C01I C 0.4686(12) 0.3441(12) 0.5592(7) 0.054(4) Uani 1 1 d . . . . .
H01Y H 0.539929 0.347038 0.580913 0.065 Uiso 1 1 calc R U . . .
HF H 0.467996 0.370554 0.505687 0.065 Uiso 1 1 calc R U . . .
C01J C 0.6046(10) 0.7439(11) 0.6459(8) 0.049(4) Uani 1 1 d . . . . .
H01S H 0.671695 0.770027 0.633777 0.059 Uiso 1 1 calc R U . . .
H01T H 0.556682 0.761087 0.600622 0.059 Uiso 1 1 calc R U . . .
C01K C 0.1036(11) 0.7483(11) 0.7742(9) 0.055(4) Uani 1 1 d . . . . .
H01O H 0.054938 0.763629 0.813936 0.066 Uiso 1 1 calc R U . . .
H01P H 0.168050 0.778259 0.776869 0.066 Uiso 1 1 calc R U . . .
C01L C 0.1456(11) 0.7404(12) 1.1091(8) 0.056(4) Uani 1 1 d . . . . .
H3 H 0.141116 0.765058 1.154728 0.067 Uiso 1 1 calc R U . . .
HG H 0.217549 0.746247 1.088192 0.067 Uiso 1 1 calc R U . . .
C01M C -0.0495(10) 0.1886(9) 0.6429(7) 0.038(3) Uani 1 1 d . . . . .
H01I H -0.008868 0.116064 0.647346 0.046 Uiso 1 1 calc R U . . .
H01J H -0.108627 0.189686 0.678158 0.046 Uiso 1 1 calc R U . . .
C01N C 0.4488(10) 0.1886(9) 0.9631(7) 0.040(3) Uani 1 1 d . . . . .
H8 H 0.387686 0.191550 0.928402 0.048 Uiso 1 1 calc R U . . .
HH H 0.488237 0.115450 0.981251 0.048 Uiso 1 1 calc R U . . .
C01O C 0.0454(13) 0.7672(11) 0.9859(7) 0.050(4) Uani 1 1 d . . . . .
H4 H -0.018974 0.811056 0.953539 0.060 Uiso 1 1 calc R U . . .
HI H 0.113520 0.770789 0.959163 0.060 Uiso 1 1 calc R U . . .
C01P C 0.3545(12) 0.2563(14) 0.6869(10) 0.074(6) Uani 1 1 d . . . . .
H01Z H 0.356338 0.228017 0.740236 0.089 Uiso 1 1 calc R U . . .
HJ H 0.283869 0.251758 0.665166 0.089 Uiso 1 1 calc R U . . .
C21 C 0.5440(10) 0.7946(9) 0.7007(7) 0.041(3) Uani 1 1 d . . . . .
H21A H 0.516988 0.869292 0.679013 0.049 Uiso 1 1 calc R U . . .
H21B H 0.595511 0.785906 0.743031 0.049 Uiso 1 1 calc R U . . .
C23 C 0.0404(10) 0.7960(10) 0.7013(7) 0.047(4) Uani 1 1 d . . . . .
H23A H 0.011683 0.870925 0.696453 0.056 Uiso 1 1 calc R U . . .
H23B H 0.091126 0.786238 0.661549 0.056 Uiso 1 1 calc R U . . .
C26 C 0.4584(13) 0.2302(11) 0.5764(8) 0.055(4) Uani 1 1 d . . . . .
H26A H 0.391550 0.225677 0.550008 0.065 Uiso 1 1 calc R U . . .
H26B H 0.524164 0.186197 0.559993 0.065 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 Br06 2.9185(12) . ?
Pb01 Br0A 3.0218(13) . ?
Pb01 Br0B 3.0632(4) . ?
Pb01 Br0D 3.0197(13) . ?
Pb01 Br0F 3.1119(13) . ?
Pb01 Br0G 3.0579(4) . ?
Pb02 Br04 2.9093(11) . ?
Pb02 Br05 2.9491(13) . ?
Pb02 Br07 3.0027(12) . ?
Pb02 Br0C 3.2208(11) 2_576 ?
Pb02 Br0E 3.2264(12) 1_554 ?
Pb02 Br0F 2.9797(13) . ?
Pb03 Br04 3.2374(11) 2_676 ?
Pb03 Br08 2.9956(13) . ?
Pb03 Br09 2.9946(13) . ?
Pb03 Br0C 2.9009(12) . ?
Pb03 Br0D 3.1945(13) . ?
Pb03 Br0E 2.9968(12) . ?
F00H C014 1.352(15) . ?
F00I C010 1.366(16) . ?
F00J C00S 1.372(15) . ?
F00K C00R 1.370(16) . ?
F1 C00W 1.396(15) . ?
F00M C019 1.354(14) . ?
F00N C014 1.381(15) . ?
F00O C00W 1.368(16) . ?
F00P C019 1.382(15) . ?
F00Q C00R 1.345(16) . ?
C00R C015 1.481(19) . ?
C00R C01I 1.51(2) . ?
C00S C00U 1.509(18) . ?
C00S F00Y 1.390(17) . ?
C00S C01J 1.494(18) . ?
F00T C010 1.361(14) . ?
C00U H00C 0.9700 . ?
C00U H00D 0.9700 . ?
C00U C017 1.49(2) . ?
C00V H00G 0.9700 . ?
C00V H00H 0.9700 . ?
C00V C019 1.500(19) . ?
C00V C01B 1.49(2) . ?
C00W C012 1.46(2) . ?
C00W C01F 1.484(17) . ?
N00X H00E 0.8900 . ?
N00X H00F 0.8900 . ?
N00X C017 1.512(16) . ?
N00X C21 1.478(16) . ?
C00Z H00A 0.9700 . ?
C00Z H00B 0.9700 . ?
C00Z N013 1.507(18) . ?
C00Z C01A 1.493(19) . ?
C010 C01A 1.52(2) . ?
C010 C01K 1.50(2) . ?
C011 H01A 0.9700 . ?
C011 H01B 0.9700 . ?
C011 C014 1.501(17) . ?
C011 C01D 1.53(2) . ?
C012 H01 0.9700 . ?
C012 H 0.9700 . ?
C012 C01L 1.50(2) . ?
N013 H01K 0.8900 . ?
N013 H01L 0.8900 . ?
N013 C23 1.478(17) . ?
C014 C01E 1.522(16) . ?
C015 H01U 0.9700 . ?
C015 H01V 0.9700 . ?
C015 C01P 1.54(2) . ?
N016 H01C 0.8900 . ?
N016 H01D 0.8900 . ?
N016 C01D 1.474(18) . ?
N016 C01M 1.449(15) . ?
C017 H01Q 0.9700 . ?
C017 H01R 0.9700 . ?
N018 H1 0.8900 . ?
N018 HA 0.8900 . ?
N018 C01L 1.498(15) . ?
N018 C01O 1.501(18) . ?
C019 C01H 1.513(16) . ?
C01A H01M 0.9700 . ?
C01A H01N 0.9700 . ?
C01B H5 0.9700 . ?
C01B HB 0.9700 . ?
C01B N01C 1.515(17) . ?
N01C H6 0.8900 . ?
N01C HC 0.8900 . ?
N01C C01N 1.447(17) . ?
C01D H01E 0.9700 . ?
C01D H01F 0.9700 . ?
C01E H01G 0.9700 . ?
C01E H01H 0.9700 . ?
C01E C01M 1.504(17) . ?
C01F H2 0.9700 . ?
C01F HD 0.9700 . ?
C01F C01O 1.485(19) . ?
N01G H01W 0.8900 . ?
N01G H01X 0.8900 . ?
N01G C01P 1.47(2) . ?
N01G C26 1.433(17) . ?
C01H H7 0.9700 . ?
C01H HE 0.9700 . ?
C01H C01N 1.476(18) . ?
C01I H01Y 0.9700 . ?
C01I HF 0.9700 . ?
C01I C26 1.53(2) . ?
C01J H01S 0.9700 . ?
C01J H01T 0.9700 . ?
C01J C21 1.453(19) . ?
C01K H01O 0.9700 . ?
C01K H01P 0.9700 . ?
C01K C23 1.481(19) . ?
C01L H3 0.9700 . ?
C01L HG 0.9700 . ?
C01M H01I 0.9700 . ?
C01M H01J 0.9700 . ?
C01N H8 0.9700 . ?
C01N HH 0.9700 . ?
C01O H4 0.9700 . ?
C01O HI 0.9700 . ?
C01P H01Z 0.9700 . ?
C01P HJ 0.9700 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C26 H26A 0.9700 . ?
C26 H26B 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
Br06 Pb01 Br0A 168.02(4) . . ?
Br06 Pb01 Br0B 86.68(3) . . ?
Br06 Pb01 Br0D 88.07(4) . . ?
Br06 Pb01 Br0F 92.21(4) . . ?
Br06 Pb01 Br0G 91.84(3) . . ?
Br0A Pb01 Br0B 82.14(3) . . ?
Br0A Pb01 Br0F 90.97(4) . . ?
Br0A Pb01 Br0G 99.99(3) . . ?
Br0B Pb01 Br0F 84.43(3) . . ?
Br0D Pb01 Br0A 89.80(4) . . ?
Br0D Pb01 Br0B 100.70(3) . . ?
Br0D Pb01 Br0F 174.87(4) . . ?
Br0D Pb01 Br0G 91.32(3) . . ?
Br0G Pb01 Br0B 167.828(14) . . ?
Br0G Pb01 Br0F 83.55(3) . . ?
Br04 Pb02 Br05 86.89(3) . . ?
Br04 Pb02 Br07 88.54(3) . . ?
Br04 Pb02 Br0C 164.99(4) . 2_576 ?
Br04 Pb02 Br0E 87.37(4) . 1_554 ?
Br04 Pb02 Br0F 96.53(4) . . ?
Br05 Pb02 Br07 166.17(4) . . ?
Br05 Pb02 Br0C 90.62(3) . 2_576 ?
Br05 Pb02 Br0E 89.29(4) . 1_554 ?
Br05 Pb02 Br0F 85.54(4) . . ?
Br07 Pb02 Br0C 97.06(3) . 2_576 ?
Br07 Pb02 Br0E 103.54(4) . 1_554 ?
Br0C Pb02 Br0E 77.79(4) 2_576 1_554 ?
Br0F Pb02 Br07 82.02(4) . . ?
Br0F Pb02 Br0C 98.03(4) . 2_576 ?
Br0F Pb02 Br0E 173.33(4) . 1_554 ?
Br08 Pb03 Br04 95.91(3) . 2_676 ?
Br08 Pb03 Br0D 103.50(4) . . ?
Br08 Pb03 Br0E 82.09(4) . . ?
Br09 Pb03 Br04 80.60(3) . 2_676 ?
Br09 Pb03 Br08 167.53(4) . . ?
Br09 Pb03 Br0D 87.72(3) . . ?
Br09 Pb03 Br0E 86.94(4) . . ?
Br0C Pb03 Br04 166.44(4) . 2_676 ?
Br0C Pb03 Br08 89.16(3) . . ?
Br0C Pb03 Br09 96.95(4) . . ?
Br0C Pb03 Br0D 87.03(4) . . ?
Br0C Pb03 Br0E 90.81(4) . . ?
Br0D Pb03 Br04 79.56(3) . 2_676 ?
Br0E Pb03 Br04 102.32(4) . 2_676 ?
Br0E Pb03 Br0D 173.96(4) . . ?
Pb02 Br04 Pb03 177.17(4) . 2_676 ?
Pb01 Br0B Pb01 180.0 . 2_576 ?
Pb03 Br0C Pb02 177.43(5) . 2_576 ?
Pb01 Br0D Pb03 171.18(5) . . ?
Pb03 Br0E Pb02 168.32(6) . 1_556 ?
Pb02 Br0F Pb01 177.09(6) . . ?
Pb01 Br0G Pb01 180.0 2_676 . ?
F00K C00R C015 108.8(12) . . ?
F00K C00R C01I 110.9(12) . . ?
F00Q C00R F00K 104.4(10) . . ?
F00Q C00R C015 109.7(13) . . ?
F00Q C00R C01I 109.6(13) . . ?
C015 C00R C01I 113.2(11) . . ?
F00J C00S C00U 107.5(10) . . ?
F00J C00S F00Y 103.7(10) . . ?
F00J C00S C01J 110.7(12) . . ?
F00Y C00S C00U 106.7(12) . . ?
F00Y C00S C01J 113.1(11) . . ?
C01J C00S C00U 114.5(10) . . ?
C00S C00U H00C 109.7 . . ?
C00S C00U H00D 109.7 . . ?
H00C C00U H00D 108.2 . . ?
C017 C00U C00S 109.8(12) . . ?
C017 C00U H00C 109.7 . . ?
C017 C00U H00D 109.7 . . ?
H00G C00V H00H 108.1 . . ?
C019 C00V H00G 109.5 . . ?
C019 C00V H00H 109.5 . . ?
C01B C00V H00G 109.5 . . ?
C01B C00V H00H 109.5 . . ?
C01B C00V C019 110.7(14) . . ?
F1 C00W C012 108.1(13) . . ?
F1 C00W C01F 109.5(10) . . ?
F00O C00W F1 103.2(11) . . ?
F00O C00W C012 110.6(12) . . ?
F00O C00W C01F 110.0(13) . . ?
C012 C00W C01F 114.8(12) . . ?
H00E N00X H00F 108.0 . . ?
C017 N00X H00E 109.4 . . ?
C017 N00X H00F 109.4 . . ?
C21 N00X H00E 109.4 . . ?
C21 N00X H00F 109.4 . . ?
C21 N00X C017 111.0(9) . . ?
H00A C00Z H00B 108.1 . . ?
N013 C00Z H00A 109.6 . . ?
N013 C00Z H00B 109.6 . . ?
C01A C00Z H00A 109.6 . . ?
C01A C00Z H00B 109.6 . . ?
C01A C00Z N013 110.2(12) . . ?
F00I C010 C01A 107.8(12) . . ?
F00I C010 C01K 113.1(12) . . ?
F00T C010 F00I 103.5(10) . . ?
F00T C010 C01A 108.4(12) . . ?
F00T C010 C01K 110.9(13) . . ?
C01K C010 C01A 112.7(11) . . ?
H01A C011 H01B 108.3 . . ?
C014 C011 H01A 109.8 . . ?
C014 C011 H01B 109.8 . . ?
C014 C011 C01D 109.2(11) . . ?
C01D C011 H01A 109.8 . . ?
C01D C011 H01B 109.8 . . ?
C00W C012 H01 109.1 . . ?
C00W C012 H 109.1 . . ?
C00W C012 C01L 112.7(12) . . ?
H01 C012 H 107.8 . . ?
C01L C012 H01 109.1 . . ?
C01L C012 H 109.1 . . ?
C00Z N013 H01K 109.4 . . ?
C00Z N013 H01L 109.4 . . ?
H01K N013 H01L 108.0 . . ?
C23 N013 C00Z 111.0(10) . . ?
C23 N013 H01K 109.4 . . ?
C23 N013 H01L 109.4 . . ?
F00H C014 F00N 105.8(11) . . ?
F00H C014 C011 110.2(10) . . ?
F00H C014 C01E 109.8(10) . . ?
F00N C014 C011 109.1(11) . . ?
F00N C014 C01E 107.9(9) . . ?
C011 C014 C01E 113.7(11) . . ?
C00R C015 H01U 109.7 . . ?
C00R C015 H01V 109.7 . . ?
C00R C015 C01P 109.7(13) . . ?
H01U C015 H01V 108.2 . . ?
C01P C015 H01U 109.7 . . ?
C01P C015 H01V 109.7 . . ?
H01C N016 H01D 107.7 . . ?
C01D N016 H01C 108.8 . . ?
C01D N016 H01D 108.8 . . ?
C01M N016 H01C 108.8 . . ?
C01M N016 H01D 108.8 . . ?
C01M N016 C01D 113.6(11) . . ?
C00U C017 N00X 108.9(10) . . ?
C00U C017 H01Q 109.9 . . ?
C00U C017 H01R 109.9 . . ?
N00X C017 H01Q 109.9 . . ?
N00X C017 H01R 109.9 . . ?
H01Q C017 H01R 108.3 . . ?
H1 N018 HA 107.8 . . ?
C01L N018 H1 109.1 . . ?
C01L N018 HA 109.1 . . ?
C01L N018 C01O 112.5(10) . . ?
C01O N018 H1 109.1 . . ?
C01O N018 HA 109.1 . . ?
F00M C019 F00P 102.7(9) . . ?
F00M C019 C00V 108.7(10) . . ?
F00M C019 C01H 110.4(11) . . ?
F00P C019 C00V 108.4(12) . . ?
F00P C019 C01H 109.5(10) . . ?
C00V C019 C01H 116.3(10) . . ?
C00Z C01A C010 109.4(11) . . ?
C00Z C01A H01M 109.8 . . ?
C00Z C01A H01N 109.8 . . ?
C010 C01A H01M 109.8 . . ?
C010 C01A H01N 109.8 . . ?
H01M C01A H01N 108.2 . . ?
C00V C01B H5 109.4 . . ?
C00V C01B HB 109.4 . . ?
C00V C01B N01C 111.0(10) . . ?
H5 C01B HB 108.0 . . ?
N01C C01B H5 109.4 . . ?
N01C C01B HB 109.4 . . ?
C01B N01C H6 109.0 . . ?
C01B N01C HC 109.0 . . ?
H6 N01C HC 107.8 . . ?
C01N N01C C01B 113.0(10) . . ?
C01N N01C H6 109.0 . . ?
C01N N01C HC 109.0 . . ?
C011 C01D H01E 109.7 . . ?
C011 C01D H01F 109.7 . . ?
N016 C01D C011 109.8(10) . . ?
N016 C01D H01E 109.7 . . ?
N016 C01D H01F 109.7 . . ?
H01E C01D H01F 108.2 . . ?
C014 C01E H01G 109.4 . . ?
C014 C01E H01H 109.4 . . ?
H01G C01E H01H 108.0 . . ?
C01M C01E C014 111.3(9) . . ?
C01M C01E H01G 109.4 . . ?
C01M C01E H01H 109.4 . . ?
C00W C01F H2 109.5 . . ?
C00W C01F HD 109.5 . . ?
C00W C01F C01O 110.6(12) . . ?
H2 C01F HD 108.1 . . ?
C01O C01F H2 109.5 . . ?
C01O C01F HD 109.5 . . ?
H01W N01G H01X 107.5 . . ?
C01P N01G H01W 108.5 . . ?
C01P N01G H01X 108.5 . . ?
C26 N01G H01W 108.5 . . ?
C26 N01G H01X 108.5 . . ?
C26 N01G C01P 115.0(11) . . ?
C019 C01H H7 109.6 . . ?
C019 C01H HE 109.6 . . ?
H7 C01H HE 108.2 . . ?
C01N C01H C019 110.1(10) . . ?
C01N C01H H7 109.6 . . ?
C01N C01H HE 109.6 . . ?
C00R C01I H01Y 109.6 . . ?
C00R C01I HF 109.6 . . ?
C00R C01I C26 110.5(12) . . ?
H01Y C01I HF 108.1 . . ?
C26 C01I H01Y 109.6 . . ?
C26 C01I HF 109.6 . . ?
C00S C01J H01S 109.5 . . ?
C00S C01J H01T 109.5 . . ?
H01S C01J H01T 108.1 . . ?
C21 C01J C00S 110.8(11) . . ?
C21 C01J H01S 109.5 . . ?
C21 C01J H01T 109.5 . . ?
C010 C01K H01O 109.6 . . ?
C010 C01K H01P 109.6 . . ?
H01O C01K H01P 108.1 . . ?
C23 C01K C010 110.2(13) . . ?
C23 C01K H01O 109.6 . . ?
C23 C01K H01P 109.6 . . ?
C012 C01L H3 109.5 . . ?
C012 C01L HG 109.5 . . ?
N018 C01L C012 110.6(11) . . ?
N018 C01L H3 109.5 . . ?
N018 C01L HG 109.5 . . ?
H3 C01L HG 108.1 . . ?
N016 C01M C01E 110.3(10) . . ?
N016 C01M H01I 109.6 . . ?
N016 C01M H01J 109.6 . . ?
C01E C01M H01I 109.6 . . ?
C01E C01M H01J 109.6 . . ?
H01I C01M H01J 108.1 . . ?
N01C C01N C01H 113.7(11) . . ?
N01C C01N H8 108.8 . . ?
N01C C01N HH 108.8 . . ?
C01H C01N H8 108.8 . . ?
C01H C01N HH 108.8 . . ?
H8 C01N HH 107.7 . . ?
N018 C01O H4 109.5 . . ?
N018 C01O HI 109.5 . . ?
C01F C01O N018 110.5(10) . . ?
C01F C01O H4 109.5 . . ?
C01F C01O HI 109.5 . . ?
H4 C01O HI 108.1 . . ?
C015 C01P H01Z 109.6 . . ?
C015 C01P HJ 109.6 . . ?
N01G C01P C015 110.1(12) . . ?
N01G C01P H01Z 109.7 . . ?
N01G C01P HJ 109.6 . . ?
H01Z C01P HJ 108.2 . . ?
N00X C21 H21A 109.2 . . ?
N00X C21 H21B 109.2 . . ?
C01J C21 N00X 111.8(11) . . ?
C01J C21 H21A 109.2 . . ?
C01J C21 H21B 109.2 . . ?
H21A C21 H21B 107.9 . . ?
N013 C23 C01K 111.1(10) . . ?
N013 C23 H23A 109.4 . . ?
N013 C23 H23B 109.4 . . ?
C01K C23 H23A 109.4 . . ?
C01K C23 H23B 109.4 . . ?
H23A C23 H23B 108.0 . . ?
N01G C26 C01I 109.1(12) . . ?
N01G C26 H26A 109.8 . . ?
N01G C26 H26B 109.9 . . ?
C01I C26 H26A 109.9 . . ?
C01I C26 H26B 109.8 . . ?
H26A C26 H26B 108.3 . . ?

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
F00H C014 C01E C01M 72.6(13) . . . . ?
F00I C010 C01A C00Z -70.6(14) . . . . ?
F00I C010 C01K C23 67.7(15) . . . . ?
F00J C00S C00U C017 70.6(13) . . . . ?
F00J C00S C01J C21 -70.4(13) . . . . ?
F00K C00R C015 C01P 70.4(14) . . . . ?
F00K C00R C01I C26 -67.8(13) . . . . ?
F1 C00W C012 C01L 71.4(14) . . . . ?
F1 C00W C01F C01O -68.3(15) . . . . ?
F00M C019 C01H C01N -76.4(12) . . . . ?
F00N C014 C01E C01M -172.6(10) . . . . ?
F00O C00W C012 C01L -176.4(11) . . . . ?
F00O C00W C01F C01O 179.0(11) . . . . ?
F00P C019 C01H C01N 171.3(11) . . . . ?
F00Q C00R C015 C01P -176.0(12) . . . . ?
F00Q C00R C01I C26 177.6(11) . . . . ?
C00R C015 C01P N01G 52.7(16) . . . . ?
C00R C01I C26 N01G -54.7(15) . . . . ?
C00S C00U C017 N00X 55.5(13) . . . . ?
C00S C01J C21 N00X -53.7(14) . . . . ?
F00T C010 C01A C00Z 178.0(12) . . . . ?
F00T C010 C01K C23 -176.6(11) . . . . ?
C00U C00S C01J C21 51.2(16) . . . . ?
C00V C019 C01H C01N 48.0(16) . . . . ?
C00V C01B N01C C01N -55.6(16) . . . . ?
C00W C012 C01L N018 49.9(16) . . . . ?
C00W C01F C01O N018 -54.8(15) . . . . ?
F00Y C00S C00U C017 -178.7(9) . . . . ?
F00Y C00S C01J C21 173.7(11) . . . . ?
C00Z N013 C23 C01K -59.0(15) . . . . ?
C010 C01K C23 N013 56.3(15) . . . . ?
C011 C014 C01E C01M -51.4(15) . . . . ?
C012 C00W C01F C01O 53.5(16) . . . . ?
N013 C00Z C01A C010 -55.7(15) . . . . ?
C014 C011 C01D N016 -55.0(15) . . . . ?
C014 C01E C01M N016 52.4(14) . . . . ?
C015 C00R C01I C26 54.8(16) . . . . ?
C017 N00X C21 C01J 59.8(13) . . . . ?
C019 C00V C01B N01C 50.8(15) . . . . ?
C019 C01H C01N N01C -50.3(13) . . . . ?
C01A C00Z N013 C23 59.0(14) . . . . ?
C01A C010 C01K C23 -54.9(15) . . . . ?
C01B C00V C019 F00M 75.7(13) . . . . ?
C01B C00V C019 F00P -173.4(10) . . . . ?
C01B C00V C019 C01H -49.5(16) . . . . ?
C01B N01C C01N C01H 55.9(14) . . . . ?
C01D C011 C014 F00H -71.6(14) . . . . ?
C01D C011 C014 F00N 172.7(11) . . . . ?
C01D C011 C014 C01E 52.2(15) . . . . ?
C01D N016 C01M C01E -58.9(14) . . . . ?
C01F C00W C012 C01L -51.2(17) . . . . ?
C01I C00R C015 C01P -53.4(16) . . . . ?
C01J C00S C00U C017 -52.8(15) . . . . ?
C01K C010 C01A C00Z 54.9(16) . . . . ?
C01L N018 C01O C01F 56.8(15) . . . . ?
C01M N016 C01D C011 60.6(15) . . . . ?
C01O N018 C01L C012 -53.5(15) . . . . ?
C01P N01G C26 C01I 58.5(17) . . . . ?
C21 N00X C017 C00U -60.2(14) . . . . ?
C26 N01G C01P C015 -57.9(17) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
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Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.787
_oxdiff_exptl_absorpt_empirical_full_min 0.440
# start Validation Reply Form
_vrf_PLAT097_hxq_211027_2_auto   
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PROBLEM: Large Reported Max.  (Positive) Residual Density       9.39 eA-3  
RESPONSE: These alerts are generated because there is a large amount of disorder
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# end Validation Reply Form
