# Supplementary Information (SI) for Materials 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_yangh2_1208_auto
_database_code_depnum_ccdc_archive 'CCDC 2339434'
loop_
_audit_author_name
_audit_author_address
'yang huan'
;lanzhou university 
China
;
_audit_update_record             
;
2024-03-11 deposited with the CCDC.	2024-11-14 downloaded from the CCDC.
;
_audit_creation_date             2023-12-08
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br4 Pb, C5 H14 N2'
_chemical_formula_sum            'C5 H14 Br4 N2 Pb'
_chemical_formula_weight         629.01
_chemical_absolute_configuration ad
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   8.7802(2)
_cell_length_b                   10.8321(3)
_cell_length_c                   13.9609(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1327.79(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6315
_cell_measurement_temperature    300.67(10)
_cell_measurement_theta_max      30.7280
_cell_measurement_theta_min      2.3720
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    24.704
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.27462
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.93a (Rigaku Oxford Diffraction, 2023)
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    3.147
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9538
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         2.740
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      300.67(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     -4.00  37.00   0.50    1.00    --    4.05 -99.00-180.00   82
  2  ω    -18.00  11.00   0.50    1.00    --    4.05 -99.00 -90.00   58
  3  ω    -36.00  16.00   0.50    1.00    --   -6.24 -78.00 -47.00  104
  4  ω    -12.00  27.00   0.50    1.00    --    4.05 -99.00  60.00   78
  5  ω    -10.00  16.00   0.50    1.00    --    4.05 -44.00 132.00   52
  6  ω    -65.00 -29.00   0.50    1.00    --    4.05 -44.00 132.00   72
;
_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      0.0659626000
_diffrn_orient_matrix_UB_12      0.0313625000
_diffrn_orient_matrix_UB_13      0.0163561000
_diffrn_orient_matrix_UB_21      0.0175723000
_diffrn_orient_matrix_UB_22      0.0170998000
_diffrn_orient_matrix_UB_23      -0.0477957000
_diffrn_orient_matrix_UB_31      -0.0431754000
_diffrn_orient_matrix_UB_32      0.0548696000
_diffrn_orient_matrix_UB_33      0.0055524000
_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         0.725
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                2550
_reflns_number_total             2707
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.224
_refine_diff_density_min         -2.660
_refine_diff_density_rms         0.368
_refine_ls_abs_structure_details 
;
 Flack x determined using 1000 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.012(8)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         2707
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0341
_refine_ls_restrained_S_all      1.095
_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)+(0.0499P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0795
_refine_ls_wR_factor_ref         0.0804
_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, All N(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C4(H008)
2.b Secondary CH2 refined with riding coordinates:
 N1(H00A,H00B), C1(H00C,H00D), C5(H00E,H00F), C3(H00J,H00K), C2(H00L,H00M)
2.c Idealised Me refined as rotating group:
 N2(H00G,H00H,H00I)
;
_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 0.30263(5) 1.21336(4) 0.48293(3) 0.02637(15) Uani 1 1 d . . . . .
Br02 Br 0.00749(14) 1.07639(12) 0.45383(10) 0.0315(3) Uani 1 1 d . . . . .
Br03 Br 0.31292(16) 1.08244(11) 0.66860(9) 0.0316(3) Uani 1 1 d . . . . .
Br04 Br 0.29906(15) 1.26323(10) 0.26568(10) 0.0322(3) Uani 1 1 d . . . . .
Br05 Br 0.56921(15) 1.06417(14) 0.44155(10) 0.0376(3) Uani 1 1 d . . . . .
N006 N 0.0603(11) 0.6701(9) 0.2949(7) 0.024(2) Uani 1 1 d . . . . .
H00A H -0.029224 0.635758 0.281346 0.029 Uiso 1 1 calc R U . . .
H00B H 0.077449 0.728918 0.251690 0.029 Uiso 1 1 calc R U . . .
C007 C 0.1808(13) 0.5750(11) 0.2866(9) 0.028(3) Uani 1 1 d . . . . .
H00C H 0.182817 0.541833 0.222089 0.033 Uiso 1 1 calc R U . . .
H00D H 0.160905 0.507869 0.330802 0.033 Uiso 1 1 calc R U . . .
C008 C 0.3331(11) 0.6353(10) 0.3101(9) 0.021(2) Uani 1 1 d . . . . .
H008 H 0.350870 0.700599 0.262803 0.025 Uiso 1 1 calc R U . . .
C009 C 0.0522(13) 0.7274(12) 0.3917(9) 0.030(3) Uani 1 1 d . . . . .
H00E H 0.025891 0.665032 0.438730 0.036 Uiso 1 1 calc R U . . .
H00F H -0.026787 0.790070 0.392401 0.036 Uiso 1 1 calc R U . . .
N00A N 0.4574(11) 0.5433(9) 0.3002(9) 0.031(2) Uani 1 1 d . . . . .
H00G H 0.453979 0.509843 0.241978 0.038 Uiso 1 1 calc R U . . .
H00H H 0.445895 0.484429 0.344069 0.038 Uiso 1 1 calc R U . . .
H00I H 0.546834 0.580400 0.308536 0.038 Uiso 1 1 calc R U . . .
C00B C 0.2030(16) 0.7852(12) 0.4177(9) 0.035(3) Uani 1 1 d . . . . .
H00J H 0.198767 0.814732 0.483265 0.042 Uiso 1 1 calc R U . . .
H00K H 0.221496 0.855633 0.376420 0.042 Uiso 1 1 calc R U . . .
C00C C 0.3340(14) 0.6939(13) 0.4077(9) 0.032(3) Uani 1 1 d . . . . .
H00L H 0.429942 0.736467 0.417548 0.039 Uiso 1 1 calc R U . . .
H00M H 0.324854 0.630341 0.456311 0.039 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 Br02 3.0136(13) . ?
Pb01 Br02 3.0334(13) 4_576 ?
Pb01 Br03 2.9560(13) . ?
Pb01 Br04 3.0810(14) . ?
Pb01 Br05 2.9023(14) . ?
N006 H00A 0.8900 . ?
N006 H00B 0.8900 . ?
N006 C007 1.481(15) . ?
N006 C009 1.490(16) . ?
C007 H00C 0.9700 . ?
C007 H00D 0.9700 . ?
C007 C008 1.523(16) . ?
C008 H008 0.9800 . ?
C008 N00A 1.485(14) . ?
C008 C00C 1.504(17) . ?
C009 H00E 0.9700 . ?
C009 H00F 0.9700 . ?
C009 C00B 1.509(19) . ?
N00A H00G 0.8900 . ?
N00A H00H 0.8900 . ?
N00A H00I 0.8900 . ?
C00B H00J 0.9700 . ?
C00B H00K 0.9700 . ?
C00B C00C 1.523(18) . ?
C00C H00L 0.9700 . ?
C00C H00M 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
Br02 Pb01 Br02 156.75(4) . 4_576 ?
Br02 Pb01 Br04 99.26(4) 4_576 . ?
Br02 Pb01 Br04 86.84(4) . . ?
Br03 Pb01 Br02 94.98(4) . 4_576 ?
Br03 Pb01 Br02 84.74(4) . . ?
Br03 Pb01 Br04 161.38(4) . . ?
Br05 Pb01 Br02 89.87(4) . 4_576 ?
Br05 Pb01 Br02 113.11(4) . . ?
Br05 Pb01 Br03 83.27(4) . . ?
Br05 Pb01 Br04 84.83(4) . . ?
Pb01 Br02 Pb01 95.80(4) . 4_476 ?
H00A N006 H00B 107.7 . . ?
C007 N006 H00A 108.9 . . ?
C007 N006 H00B 108.9 . . ?
C007 N006 C009 113.3(9) . . ?
C009 N006 H00A 108.9 . . ?
C009 N006 H00B 108.9 . . ?
N006 C007 H00C 110.1 . . ?
N006 C007 H00D 110.1 . . ?
N006 C007 C008 108.2(9) . . ?
H00C C007 H00D 108.4 . . ?
C008 C007 H00C 110.1 . . ?
C008 C007 H00D 110.1 . . ?
C007 C008 H008 107.7 . . ?
N00A C008 C007 109.7(9) . . ?
N00A C008 H008 107.7 . . ?
N00A C008 C00C 111.3(10) . . ?
C00C C008 C007 112.4(10) . . ?
C00C C008 H008 107.7 . . ?
N006 C009 H00E 109.6 . . ?
N006 C009 H00F 109.6 . . ?
N006 C009 C00B 110.4(9) . . ?
H00E C009 H00F 108.1 . . ?
C00B C009 H00E 109.6 . . ?
C00B C009 H00F 109.6 . . ?
C008 N00A H00G 109.5 . . ?
C008 N00A H00H 109.5 . . ?
C008 N00A H00I 109.5 . . ?
H00G N00A H00H 109.5 . . ?
H00G N00A H00I 109.5 . . ?
H00H N00A H00I 109.5 . . ?
C009 C00B H00J 109.3 . . ?
C009 C00B H00K 109.3 . . ?
C009 C00B C00C 111.8(10) . . ?
H00J C00B H00K 107.9 . . ?
C00C C00B H00J 109.3 . . ?
C00C C00B H00K 109.3 . . ?
C008 C00C C00B 110.7(10) . . ?
C008 C00C H00L 109.5 . . ?
C008 C00C H00M 109.5 . . ?
C00B C00C H00L 109.5 . . ?
C00B C00C H00M 109.5 . . ?
H00L C00C H00M 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
N006 C007 C008 N00A -178.6(11) . . . . ?
N006 C007 C008 C00C 56.9(13) . . . . ?
N006 C009 C00B C00C -53.3(14) . . . . ?
C007 N006 C009 C00B 57.9(13) . . . . ?
C007 C008 C00C C00B -54.8(14) . . . . ?
C009 N006 C007 C008 -58.6(13) . . . . ?
C009 C00B C00C C008 52.5(15) . . . . ?
N00A C008 C00C C00B -178.3(10) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.524
_oxdiff_exptl_absorpt_empirical_full_min 0.574
####################################################################### 
# 
# 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_yanghuan1-zhhl_1215-1_auto
_database_code_depnum_ccdc_archive 'CCDC 2339435'
loop_
_audit_author_name
_audit_author_address
'yang huan'
;lanzhou university 
China
;
_audit_update_record             
;
2024-03-11 deposited with the CCDC.	2024-11-14 downloaded from the CCDC.
;
_audit_creation_date             2023-12-15
_audit_creation_method           
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br4 Pb, C5 H14 N2'
_chemical_formula_sum            'C5 H14 Br4 N2 Pb'
_chemical_formula_weight         629.01
_chemical_absolute_configuration ad
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   8.7810(3)
_cell_length_b                   10.8005(4)
_cell_length_c                   13.7783(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1306.72(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6845
_cell_measurement_temperature    149.97(10)
_cell_measurement_theta_max      30.8160
_cell_measurement_theta_min      2.3090
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    25.103
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.12106
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.93a (Rigaku Oxford Diffraction, 2023)
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    3.197
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0954
_diffrn_reflns_av_unetI/netI     0.0834
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.847
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9815
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.810
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.416
_diffrn_reflns_theta_min         2.396
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.97(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.847
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      3.00  28.00   0.50    0.34    --    4.05  37.00 -90.00   50
  2  ω     34.00  61.00   0.50    0.34    --    4.05  37.00 -90.00   54
  3  ω    -12.00  35.00   0.50    0.34    --    4.05 -99.00-180.00   94
  4  ω    -65.00  15.00   0.50    0.34    --    4.05 -73.00 -69.00  160
  5  ω    -18.00  37.00   0.50    0.34    --    4.05 -99.00  30.00  110
;
_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      0.0650990000
_diffrn_orient_matrix_UB_12      0.0192200000
_diffrn_orient_matrix_UB_13      0.0264802000
_diffrn_orient_matrix_UB_21      -0.0053607000
_diffrn_orient_matrix_UB_22      0.0596374000
_diffrn_orient_matrix_UB_23      -0.0212882000
_diffrn_orient_matrix_UB_31      -0.0475547000
_diffrn_orient_matrix_UB_32      0.0196624000
_diffrn_orient_matrix_UB_33      0.0386607000
_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         0.677
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.761
_reflns_number_gt                2817
_reflns_number_total             3208
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         6.725
_refine_diff_density_min         -4.703
_refine_diff_density_rms         0.623
_refine_ls_abs_structure_details 
;
 Flack x determined using 960 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.02(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.170
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         3208
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.0797
_refine_ls_R_factor_gt           0.0711
_refine_ls_restrained_S_all      1.163
_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)+(0.1210P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1867
_refine_ls_wR_factor_ref         0.1925
_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, All N(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C2) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(C5) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma
of 0.004 and sigma for terminal atoms of 0.002
3.a Ternary CH refined with riding coordinates:
 C4(H4)
3.b Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C1(H1C,H1D), C2(H2D,H2E), C3(H3A,H3B), C5(H5A,H5B)
3.c Idealised Me refined as rotating group:
 N2(H2A,H2B,H2C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.19607(11) 0.78575(8) 0.51842(6) 0.0143(3) Uani 1 1 d . . . . .
Br1 Br -0.0075(3) 0.5760(2) 0.45336(18) 0.0164(5) Uani 1 1 d . . . . .
Br2 Br 0.1855(3) 0.9157(2) 0.33077(17) 0.0174(5) Uani 1 1 d . . . . .
Br3 Br -0.0715(3) 0.9340(2) 0.55940(18) 0.0195(6) Uani 1 1 d . . . . .
Br4 Br 0.1997(3) 0.7371(2) 0.73889(18) 0.0185(5) Uani 1 1 d . . . . .
N1 N 0.060(2) 0.667(2) 0.2039(14) 0.015(4) Uani 1 1 d . U . . .
H1A H -0.031800 0.632466 0.217918 0.018 Uiso 1 1 calc R U . . .
H1B H 0.078835 0.726645 0.249067 0.018 Uiso 1 1 calc R U . . .
N2 N 0.460(3) 0.542(2) 0.1964(16) 0.020(5) Uani 1 1 d . U . . .
H2A H 0.444059 0.480825 0.152224 0.024 Uiso 1 1 calc R U . . .
H2B H 0.461998 0.509045 0.257162 0.024 Uiso 1 1 calc R U . . .
H2C H 0.550431 0.579919 0.183887 0.024 Uiso 1 1 calc R U . . .
C1 C 0.180(3) 0.570(2) 0.2105(16) 0.014(4) Uani 1 1 d . U . . .
H1C H 0.161458 0.504285 0.162120 0.017 Uiso 1 1 calc R U . . .
H1D H 0.180928 0.532855 0.275997 0.017 Uiso 1 1 calc R U . . .
C2 C 0.052(3) 0.726(2) 0.1065(17) 0.017(5) Uani 1 1 d . U . . .
H2D H 0.027336 0.662023 0.057263 0.020 Uiso 1 1 calc R U . . .
H2E H -0.029640 0.788646 0.105867 0.020 Uiso 1 1 calc R U . . .
C3 C 0.335(3) 0.693(2) 0.0917(16) 0.016(5) Uani 1 1 d . U . . .
H3A H 0.327647 0.628393 0.041346 0.019 Uiso 1 1 calc R U . . .
H3B H 0.432281 0.738427 0.082177 0.019 Uiso 1 1 calc R U . . .
C4 C 0.333(3) 0.636(2) 0.1898(17) 0.014(5) Uani 1 1 d . U . . .
H4 H 0.349677 0.701414 0.239753 0.017 Uiso 1 1 calc R U . . .
C5 C 0.199(3) 0.785(2) 0.0818(18) 0.021(5) Uani 1 1 d . U . . .
H5A H 0.216200 0.856479 0.125325 0.025 Uiso 1 1 calc R U . . .
H5B H 0.194970 0.816074 0.014363 0.025 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br1 3.026(3) 4_566 ?
Pb1 Br1 3.021(3) . ?
Pb1 Br2 2.943(2) . ?
Pb1 Br3 2.898(3) . ?
Pb1 Br4 3.083(3) . ?
N1 C1 1.49(3) . ?
N1 C2 1.48(3) . ?
N2 C4 1.51(3) . ?
C1 C4 1.54(3) . ?
C2 C5 1.48(4) . ?
C3 C4 1.49(3) . ?
C3 C5 1.55(3) . ?

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 156.47(7) . 4_566 ?
Br1 Pb1 Br4 99.83(7) . . ?
Br1 Pb1 Br4 87.05(7) 4_566 . ?
Br2 Pb1 Br1 84.54(8) . 4_566 ?
Br2 Pb1 Br1 94.49(7) . . ?
Br2 Pb1 Br4 161.28(7) . . ?
Br3 Pb1 Br1 113.56(7) . 4_566 ?
Br3 Pb1 Br1 89.57(7) . . ?
Br3 Pb1 Br2 83.23(7) . . ?
Br3 Pb1 Br4 84.87(7) . . ?
Pb1 Br1 Pb1 95.79(7) . 4_466 ?
C2 N1 C1 112.8(18) . . ?
N1 C1 C4 106.5(18) . . ?
C5 C2 N1 110.5(19) . . ?
C4 C3 C5 109.6(19) . . ?
N2 C4 C1 109.0(18) . . ?
C3 C4 N2 109.0(19) . . ?
C3 C4 C1 112(2) . . ?
C2 C5 C3 112(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 2.585
_oxdiff_exptl_absorpt_empirical_full_min 0.336
####################################################################### 
# 
# 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_yanghuan3-zhhl_1215_auto
_database_code_depnum_ccdc_archive 'CCDC 2339436'
loop_
_audit_author_name
_audit_author_address
'yang huan'
;lanzhou university 
China
;
_audit_update_record             
;
2024-03-11 deposited with the CCDC.	2024-11-14 downloaded from the CCDC.
;
_audit_creation_date             2023-12-15
_audit_creation_method           
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br6 Pb, 2(H2 O), 2(C6 H16 N2)'
_chemical_formula_sum            'C12 H36 Br6 N4 O2 Pb'
_chemical_formula_weight         955.10
_chemical_absolute_configuration ad
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   9.8774(2)
_cell_length_b                   10.8539(2)
_cell_length_c                   24.3071(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2605.92(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    14370
_cell_measurement_temperature    150.00(11)
_cell_measurement_theta_max      30.4940
_cell_measurement_theta_min      1.7060
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    15.688
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36816
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.93a (Rigaku Oxford Diffraction, 2023)
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    2.434
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.858
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            23794
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.822
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.731
_diffrn_reflns_theta_min         2.055
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(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 0.858
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -3.00  22.00   0.50    1.91    --    4.02 -86.00 133.00   50
  2  ω    -58.00   6.00   0.50    1.91    --   -6.05 -41.00 -32.00  128
  3  ω    -18.00   7.00   0.50    1.91    --    4.02 -99.00-120.00   50
  4  ω    -67.00  74.00   0.50    1.91    --    4.02   0.00-150.00  282
;
_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      -0.0267866000
_diffrn_orient_matrix_UB_12      0.0568982000
_diffrn_orient_matrix_UB_13      -0.0093492000
_diffrn_orient_matrix_UB_21      -0.0255234000
_diffrn_orient_matrix_UB_22      0.0120711000
_diffrn_orient_matrix_UB_23      0.0267450000
_diffrn_orient_matrix_UB_31      0.0615333000
_diffrn_orient_matrix_UB_32      0.0297636000
_diffrn_orient_matrix_UB_33      0.0070264000
_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         0.714
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.777
_reflns_number_gt                6210
_reflns_number_total             6672
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.691
_refine_diff_density_min         -0.633
_refine_diff_density_rms         0.128
_refine_ls_abs_structure_details 
;
 Flack x determined using 2445 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.018(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         6672
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0249
_refine_ls_R_factor_gt           0.0206
_refine_ls_restrained_S_all      1.023
_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)+(0.0131P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0330
_refine_ls_wR_factor_ref         0.0336
_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,H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O1(H1E,H1D), O2(H2D,H2E)
2.b Ternary CH refined with riding coordinates:
 C2(H2), C12(H12), C1(H1), C4(H4)
2.c Secondary CH2 refined with riding coordinates:
 C3(H3D,H3E), C6(H6A,H6B), C7(H7A,H7B), C9(H9A,H9B), C5(H5A,H5B), C8(H8A,H8B),
 C10(H10A,H10B), C11(H11A,H11B)
2.d Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N3(H3A,H3B,H3C), N2(H2A,H2B,H2C), N4(H4A,H4B,H4C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.72399(2) 1.28021(2) 0.13697(2) 0.01573(4) Uani 1 1 d . . . . .
Br1 Br 0.49370(4) 1.12475(4) 0.17954(2) 0.01746(9) Uani 1 1 d . . . . .
Br2 Br 0.70471(4) 1.14006(4) 0.02867(2) 0.02046(10) Uani 1 1 d . . . . .
Br3 Br 0.92843(4) 1.42502(4) 0.07452(2) 0.02132(10) Uani 1 1 d . . . . .
Br4 Br 0.94834(4) 1.11285(4) 0.17407(2) 0.01940(10) Uani 1 1 d . . . . .
Br5 Br 0.75596(4) 1.38740(4) 0.24959(2) 0.02238(10) Uani 1 1 d . . . . .
Br6 Br 0.50240(4) 1.46291(5) 0.10073(2) 0.02228(10) Uani 1 1 d . . . . .
O1 O 0.7455(4) 1.0957(3) 0.30604(14) 0.0291(8) Uani 1 1 d G . . . .
H1E H 0.755241 1.154732 0.282179 0.044 Uiso 1 1 d G U . . .
H1D H 0.698373 1.128511 0.332490 0.044 Uiso 1 1 d G U . . .
O2 O 0.7835(3) 0.8333(3) 0.38075(14) 0.0258(7) Uani 1 1 d G . . . .
H2D H 0.715731 0.879809 0.390319 0.039 Uiso 1 1 d G U . . .
H2E H 0.853310 0.866400 0.396781 0.039 Uiso 1 1 d G U . . .
N1 N 0.8954(3) 0.8671(4) 0.27214(17) 0.0232(9) Uani 1 1 d . . . . .
H1A H 0.899052 0.946079 0.259668 0.028 Uiso 1 1 calc R U . . .
H1B H 0.980500 0.835059 0.273251 0.028 Uiso 1 1 calc R U . . .
H1C H 0.858980 0.866066 0.306528 0.028 Uiso 1 1 calc R U . . .
N3 N 0.5955(3) 0.8946(3) 0.26595(15) 0.0160(8) Uani 1 1 d . . . . .
H3A H 0.511689 0.917570 0.254278 0.019 Uiso 1 1 calc R U . . .
H3B H 0.634320 0.957800 0.284800 0.019 Uiso 1 1 calc R U . . .
H3C H 0.588202 0.827724 0.288356 0.019 Uiso 1 1 calc R U . . .
C2 C 0.6815(4) 0.8626(4) 0.21726(18) 0.0156(9) Uani 1 1 d . . . . .
H2 H 0.710486 0.941002 0.199115 0.019 Uiso 1 1 calc R U . . .
C3 C 0.8919(5) 0.7610(5) 0.1826(2) 0.0285(12) Uani 1 1 d . . . . .
H3D H 0.928861 0.838260 0.167071 0.034 Uiso 1 1 calc R U . . .
H3E H 0.969103 0.707749 0.193050 0.034 Uiso 1 1 calc R U . . .
C6 C 0.5975(5) 0.7893(5) 0.17645(19) 0.0235(10) Uani 1 1 d . . . . .
H6A H 0.513963 0.835349 0.167293 0.028 Uiso 1 1 calc R U . . .
H6B H 0.571058 0.709489 0.192955 0.028 Uiso 1 1 calc R U . . .
C7 C 0.6798(5) 0.7670(5) 0.1244(2) 0.0329(13) Uani 1 1 d . . . . .
H7A H 0.625299 0.719514 0.097563 0.040 Uiso 1 1 calc R U . . .
H7B H 0.704450 0.846750 0.107336 0.040 Uiso 1 1 calc R U . . .
C9 C 0.8071(5) 0.6958(5) 0.1390(2) 0.0370(14) Uani 1 1 d . . . . .
H9A H 0.862507 0.684520 0.105405 0.044 Uiso 1 1 calc R U . . .
H9B H 0.781434 0.613098 0.152654 0.044 Uiso 1 1 calc R U . . .
C12 C 0.8088(4) 0.7911(4) 0.23403(18) 0.0184(9) Uani 1 1 d . . . . .
H12 H 0.781929 0.712861 0.252835 0.022 Uiso 1 1 calc R U . . .
N2 N 1.3470(3) 1.1297(4) 0.05840(17) 0.0224(9) Uani 1 1 d . . . . .
H2A H 1.373164 1.127385 0.022522 0.027 Uiso 1 1 calc R U . . .
H2B H 1.421494 1.128917 0.080413 0.027 Uiso 1 1 calc R U . . .
H2C H 1.298625 1.199653 0.064697 0.027 Uiso 1 1 calc R U . . .
N4 N 1.0488(3) 1.1228(4) 0.04018(16) 0.0214(9) Uani 1 1 d . . . . .
H4A H 0.969923 1.110741 0.021627 0.026 Uiso 1 1 calc R U . . .
H4B H 1.091368 1.190747 0.026705 0.026 Uiso 1 1 calc R U . . .
H4C H 1.030862 1.133793 0.076567 0.026 Uiso 1 1 calc R U . . .
C1 C 1.2606(4) 1.0193(4) 0.07090(19) 0.0206(10) Uani 1 1 d . . . . .
H1 H 1.228580 1.024779 0.109853 0.025 Uiso 1 1 calc R U . . .
C4 C 1.1379(4) 1.0130(4) 0.03304(19) 0.0179(10) Uani 1 1 d . . . . .
H4 H 1.170026 1.010182 -0.005957 0.021 Uiso 1 1 calc R U . . .
C5 C 1.3462(5) 0.9040(5) 0.0644(2) 0.0273(11) Uani 1 1 d . . . . .
H5A H 1.380836 0.899230 0.026220 0.033 Uiso 1 1 calc R U . . .
H5B H 1.424885 0.908379 0.089533 0.033 Uiso 1 1 calc R U . . .
C8 C 1.0556(5) 0.8979(4) 0.0448(2) 0.0274(11) Uani 1 1 d . . . . .
H8A H 0.978809 0.893419 0.018672 0.033 Uiso 1 1 calc R U . . .
H8B H 1.018069 0.902735 0.082462 0.033 Uiso 1 1 calc R U . . .
C10 C 1.2650(5) 0.7907(5) 0.0770(2) 0.0336(12) Uani 1 1 d . . . . .
H10A H 1.234922 0.793122 0.115814 0.040 Uiso 1 1 calc R U . . .
H10B H 1.322486 0.716764 0.072040 0.040 Uiso 1 1 calc R U . . .
C11 C 1.1416(5) 0.7815(5) 0.0394(2) 0.0363(13) Uani 1 1 d . . . . .
H11A H 1.086984 0.708524 0.049641 0.044 Uiso 1 1 calc R U . . .
H11B H 1.171423 0.771436 0.000786 0.044 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br1 3.0154(5) . ?
Pb1 Br2 3.0463(5) . ?
Pb1 Br3 2.9752(5) . ?
Pb1 Br4 3.0039(5) . ?
Pb1 Br5 2.9911(5) . ?
Pb1 Br6 3.0820(5) . ?
N1 C12 1.507(6) . ?
N3 C2 1.498(5) . ?
C2 C6 1.518(6) . ?
C2 C12 1.533(6) . ?
C3 C9 1.526(7) . ?
C3 C12 1.530(6) . ?
C6 C7 1.524(6) . ?
C7 C9 1.518(8) . ?
N2 C1 1.502(6) . ?
N4 C4 1.491(5) . ?
C1 C4 1.523(6) . ?
C1 C5 1.519(6) . ?
C4 C8 1.518(6) . ?
C5 C10 1.500(7) . ?
C8 C11 1.528(7) . ?
C10 C11 1.526(7) . ?

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 Br2 88.279(13) . . ?
Br1 Pb1 Br6 85.548(13) . . ?
Br2 Pb1 Br6 91.716(13) . . ?
Br3 Pb1 Br1 169.329(14) . . ?
Br3 Pb1 Br2 82.263(13) . . ?
Br3 Pb1 Br4 88.393(13) . . ?
Br3 Pb1 Br5 100.942(14) . . ?
Br3 Pb1 Br6 89.788(13) . . ?
Br4 Pb1 Br1 96.608(12) . . ?
Br4 Pb1 Br2 90.205(13) . . ?
Br4 Pb1 Br6 177.156(15) . . ?
Br5 Pb1 Br1 89.036(13) . . ?
Br5 Pb1 Br2 172.601(14) . . ?
Br5 Pb1 Br4 83.256(13) . . ?
Br5 Pb1 Br6 94.948(13) . . ?
N3 C2 C6 109.1(3) . . ?
N3 C2 C12 111.9(4) . . ?
C6 C2 C12 110.9(4) . . ?
C9 C3 C12 111.9(4) . . ?
C2 C6 C7 109.5(4) . . ?
C9 C7 C6 109.2(4) . . ?
C7 C9 C3 112.4(4) . . ?
N1 C12 C2 110.6(3) . . ?
N1 C12 C3 108.3(4) . . ?
C3 C12 C2 109.3(4) . . ?
N2 C1 C4 111.4(4) . . ?
N2 C1 C5 108.6(4) . . ?
C5 C1 C4 110.1(4) . . ?
N4 C4 C1 111.3(4) . . ?
N4 C4 C8 108.6(3) . . ?
C8 C4 C1 110.5(4) . . ?
C10 C5 C1 110.9(4) . . ?
C4 C8 C11 111.5(4) . . ?
C5 C10 C11 111.0(4) . . ?
C10 C11 C8 109.8(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 2.178
_oxdiff_exptl_absorpt_empirical_full_min 0.730
####################################################################### 
# 
# 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_exp_13171
_database_code_depnum_ccdc_archive 'CCDC 2339439'
loop_
_audit_author_name
_audit_author_address
'yang huan'
;lanzhou university 
China
;
_audit_update_record             
;
2024-03-11 deposited with the CCDC.	2024-11-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H36 Br6 N4 O2 Pb'
_chemical_formula_weight         955.10

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -4.0753 8.5060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

_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+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   9.9329(2)
_cell_length_b                   10.9337(3)
_cell_length_c                   24.3960(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2649.49(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    10130
_cell_measurement_theta_min      4.8020
_cell_measurement_theta_max      71.0660

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            RED
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.394
_exptl_crystal_F_000             1776
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    23.099
_shelx_estimated_absorpt_T_min   0.168
_shelx_estimated_absorpt_T_max   0.185
_exptl_absorpt_correction_T_min  0.01999
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16969
_diffrn_reflns_av_unetI/netI     0.0590
_diffrn_reflns_av_R_equivalents  0.0703
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         3.624
_diffrn_reflns_theta_max         67.239
_diffrn_reflns_theta_full        67.239
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4722
_reflns_number_gt                4539
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.753
_reflns_Friedel_fraction_max     0.998
_reflns_Friedel_fraction_full    0.998

_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 1.171.42.49 (Rigaku OD, 2022)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_structure_solution    'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_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)+(0.0731P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.00312(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 1841 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.054(6)
_chemical_absolute_configuration RM
_refine_ls_number_reflns         4722
_refine_ls_number_parameters     231
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0444
_refine_ls_wR_factor_ref         0.1134
_refine_ls_wR_factor_gt          0.1110
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.004
_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 0.27490(5) 0.78234(5) 0.63694(2) 0.0277(2) Uani 1 1 d . . . . .
Br1 Br 0.24510(16) 0.88941(15) 0.74883(7) 0.0432(4) Uani 1 1 d . . . . .
Br2 Br 0.05129(16) 0.61404(13) 0.67360(6) 0.0357(4) Uani 1 1 d . . . . .
Br3 Br 0.29308(17) 0.64233(14) 0.52863(6) 0.0382(4) Uani 1 1 d . . . . .
Br4 Br 0.49584(17) 0.96166(16) 0.60084(7) 0.0416(4) Uani 1 1 d . . . . .
Br5 Br 0.50427(16) 0.62736(12) 0.67944(6) 0.0319(3) Uani 1 1 d . . . . .
Br6 Br 0.06964(17) 0.92591(14) 0.57560(7) 0.0407(4) Uani 1 1 d . . . . .
N1 N 0.8955(14) 0.8696(14) 0.7271(6) 0.048(4) Uani 1 1 d . . . . .
H1A H 0.856582 0.873340 0.694288 0.073 Uiso 1 1 calc R U . . .
H1B H 0.976016 0.834609 0.724005 0.073 Uiso 1 1 calc R U . . .
H1C H 0.905051 0.944912 0.740448 0.073 Uiso 1 1 calc R U . . .
N2 N 0.5959(13) 0.8939(11) 0.7350(5) 0.034(3) Uani 1 1 d . . . . .
H2A H 0.631732 0.955650 0.716267 0.051 Uiso 1 1 calc R U . . .
H2B H 0.514608 0.915327 0.747062 0.051 Uiso 1 1 calc R U . . .
H2F H 0.588692 0.828768 0.713383 0.051 Uiso 1 1 calc R U . . .
N3 N 0.9501(13) 0.6231(11) 0.5403(5) 0.037(3) Uani 1 1 d . . . . .
H3A H 0.910382 0.688739 0.526028 0.055 Uiso 1 1 calc R U . . .
H3B H 1.027796 0.609679 0.523157 0.055 Uiso 1 1 calc R U . . .
H3E H 0.965409 0.635442 0.575793 0.055 Uiso 1 1 calc R U . . .
N4 N 0.6515(13) 0.6293(13) 0.5578(6) 0.041(3) Uani 1 1 d . . . . .
H4A H 0.600217 0.613748 0.528670 0.062 Uiso 1 1 calc R U . . .
H4B H 0.704824 0.692777 0.550592 0.062 Uiso 1 1 calc R U . . .
H4E H 0.599397 0.646737 0.586379 0.062 Uiso 1 1 calc R U . . .
O1 O 0.7438(14) 0.0976(11) 0.6950(5) 0.060(4) Uani 1 1 d . . . . .
H1F H 0.812164 0.068897 0.678487 0.072 Uiso 1 1 d R U . . .
H1E H 0.751414 0.159617 0.715797 0.072 Uiso 1 1 d R U . . .
O2 O 0.7815(13) 0.8331(12) 0.6188(5) 0.055(3) Uani 1 1 d . . . . .
H2E H 0.845868 0.853558 0.597770 0.066 Uiso 1 1 d R U . . .
H2G H 0.724388 0.890747 0.616149 0.066 Uiso 1 1 d R U . . .
C1 C 0.8078(15) 0.7944(12) 0.7658(6) 0.032(3) Uani 1 1 d . . . . .
H1 H 0.781171 0.718489 0.747403 0.039 Uiso 1 1 calc R U . . .
C2 C 0.8919(19) 0.7633(15) 0.8160(7) 0.051(5) Uani 1 1 d . . . . .
H2C H 0.967931 0.713398 0.804932 0.061 Uiso 1 1 calc R U . . .
H2D H 0.926683 0.838116 0.831922 0.061 Uiso 1 1 calc R U . . .
C3 C 0.810(3) 0.6949(17) 0.8588(7) 0.070(7) Uani 1 1 d . . . . .
H3C H 0.865683 0.680768 0.890999 0.084 Uiso 1 1 calc R U . . .
H3D H 0.783442 0.615989 0.844322 0.084 Uiso 1 1 calc R U . . .
C4 C 0.685(3) 0.7682(18) 0.8751(7) 0.069(6) Uani 1 1 d . . . . .
H4C H 0.632259 0.722642 0.901656 0.083 Uiso 1 1 calc R U . . .
H4D H 0.711143 0.845334 0.891540 0.083 Uiso 1 1 calc R U . . .
C5 C 0.6012(19) 0.7915(15) 0.8238(5) 0.044(4) Uani 1 1 d . . . . .
H5A H 0.520590 0.836724 0.833431 0.053 Uiso 1 1 calc R U . . .
H5B H 0.573967 0.714130 0.807818 0.053 Uiso 1 1 calc R U . . .
C6 C 0.6831(13) 0.8642(11) 0.7822(5) 0.025(3) Uani 1 1 d . . . . .
H6 H 0.711222 0.940986 0.799468 0.030 Uiso 1 1 calc R U . . .
C7 C 0.8586(15) 0.5123(13) 0.5332(5) 0.031(3) Uani 1 1 d . . . . .
H7 H 0.828006 0.509049 0.495052 0.038 Uiso 1 1 calc R U . . .
C8 C 0.944(2) 0.3994(15) 0.5449(8) 0.051(4) Uani 1 1 d . . . . .
H8A H 0.981042 0.404023 0.581635 0.061 Uiso 1 1 calc R U . . .
H8B H 1.018298 0.395099 0.519109 0.061 Uiso 1 1 calc R U . . .
C9 C 0.856(3) 0.2855(17) 0.5394(9) 0.070(6) Uani 1 1 d . . . . .
H9A H 0.825947 0.277550 0.501717 0.083 Uiso 1 1 calc R U . . .
H9B H 0.908318 0.213576 0.548513 0.083 Uiso 1 1 calc R U . . .
C10 C 0.735(2) 0.2919(15) 0.5765(7) 0.066(6) Uani 1 1 d . . . . .
H10A H 0.678548 0.220259 0.571075 0.080 Uiso 1 1 calc R U . . .
H10B H 0.763501 0.293108 0.614510 0.080 Uiso 1 1 calc R U . . .
C11 C 0.656(2) 0.4040(16) 0.5643(8) 0.057(5) Uani 1 1 d . . . . .
H11A H 0.578667 0.407416 0.588723 0.069 Uiso 1 1 calc R U . . .
H11B H 0.622011 0.399133 0.527078 0.069 Uiso 1 1 calc R U . . .
C12 C 0.7358(18) 0.5195(14) 0.5706(5) 0.041(4) Uani 1 1 d . . . . .
H12 H 0.766756 0.525585 0.608607 0.049 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 Br6 2.9766(17) . ?
Pb1 Br1 2.9849(16) . ?
Pb1 Br2 3.0199(16) . ?
Pb1 Br5 3.0228(15) . ?
Pb1 Br3 3.0591(16) . ?
Pb1 Br4 3.0717(17) . ?
N1 C1 1.53(2) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N2 C6 1.477(17) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 H2F 0.8900 . ?
N3 C7 1.524(18) . ?
N3 H3A 0.8900 . ?
N3 H3B 0.8900 . ?
N3 H3E 0.8900 . ?
N4 C12 1.50(2) . ?
N4 H4A 0.8900 . ?
N4 H4B 0.8900 . ?
N4 H4E 0.8900 . ?
O1 H1F 0.8499 . ?
O1 H1E 0.8500 . ?
O2 H2E 0.8498 . ?
O2 H2G 0.8500 . ?
C1 C6 1.509(18) . ?
C1 C2 1.520(19) . ?
C1 H1 0.9800 . ?
C2 C3 1.52(3) . ?
C2 H2C 0.9700 . ?
C2 H2D 0.9700 . ?
C3 C4 1.54(4) . ?
C3 H3C 0.9700 . ?
C3 H3D 0.9700 . ?
C4 C5 1.52(2) . ?
C4 H4C 0.9700 . ?
C4 H4D 0.9700 . ?
C5 C6 1.524(19) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6 0.9800 . ?
C7 C12 1.52(2) . ?
C7 C8 1.53(2) . ?
C7 H7 0.9800 . ?
C8 C9 1.53(2) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.51(3) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.48(3) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.50(2) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br6 Pb1 Br1 100.66(5) . . ?
Br6 Pb1 Br2 88.08(5) . . ?
Br1 Pb1 Br2 83.99(5) . . ?
Br6 Pb1 Br5 169.84(5) . . ?
Br1 Pb1 Br5 88.91(5) . . ?
Br2 Pb1 Br5 96.38(4) . . ?
Br6 Pb1 Br3 82.54(5) . . ?
Br1 Pb1 Br3 172.77(5) . . ?
Br2 Pb1 Br3 89.67(4) . . ?
Br5 Pb1 Br3 88.35(4) . . ?
Br6 Pb1 Br4 90.50(5) . . ?
Br1 Pb1 Br4 94.74(5) . . ?
Br2 Pb1 Br4 177.88(5) . . ?
Br5 Pb1 Br4 85.28(4) . . ?
Br3 Pb1 Br4 91.70(5) . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
H1A N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C6 N2 H2A 109.5 . . ?
C6 N2 H2B 109.5 . . ?
H2A N2 H2B 109.5 . . ?
C6 N2 H2F 109.5 . . ?
H2A N2 H2F 109.5 . . ?
H2B N2 H2F 109.5 . . ?
C7 N3 H3A 109.5 . . ?
C7 N3 H3B 109.5 . . ?
H3A N3 H3B 109.5 . . ?
C7 N3 H3E 109.5 . . ?
H3A N3 H3E 109.5 . . ?
H3B N3 H3E 109.5 . . ?
C12 N4 H4A 109.5 . . ?
C12 N4 H4B 109.5 . . ?
H4A N4 H4B 109.5 . . ?
C12 N4 H4E 109.5 . . ?
H4A N4 H4E 109.5 . . ?
H4B N4 H4E 109.5 . . ?
H1F O1 H1E 120.4 . . ?
H2E O2 H2G 105.2 . . ?
C6 C1 C2 110.5(12) . . ?
C6 C1 N1 111.1(11) . . ?
C2 C1 N1 107.8(13) . . ?
C6 C1 H1 109.1 . . ?
C2 C1 H1 109.1 . . ?
N1 C1 H1 109.1 . . ?
C3 C2 C1 111.9(16) . . ?
C3 C2 H2C 109.2 . . ?
C1 C2 H2C 109.2 . . ?
C3 C2 H2D 109.2 . . ?
C1 C2 H2D 109.2 . . ?
H2C C2 H2D 107.9 . . ?
C2 C3 C4 110.7(14) . . ?
C2 C3 H3C 109.5 . . ?
C4 C3 H3C 109.5 . . ?
C2 C3 H3D 109.5 . . ?
C4 C3 H3D 109.5 . . ?
H3C C3 H3D 108.1 . . ?
C5 C4 C3 108.6(16) . . ?
C5 C4 H4C 110.0 . . ?
C3 C4 H4C 110.0 . . ?
C5 C4 H4D 110.0 . . ?
C3 C4 H4D 110.0 . . ?
H4C C4 H4D 108.4 . . ?
C4 C5 C6 110.1(14) . . ?
C4 C5 H5A 109.6 . . ?
C6 C5 H5A 109.6 . . ?
C4 C5 H5B 109.6 . . ?
C6 C5 H5B 109.6 . . ?
H5A C5 H5B 108.2 . . ?
N2 C6 C1 112.7(11) . . ?
N2 C6 C5 108.7(12) . . ?
C1 C6 C5 110.6(12) . . ?
N2 C6 H6 108.2 . . ?
C1 C6 H6 108.2 . . ?
C5 C6 H6 108.2 . . ?
N3 C7 C12 111.6(12) . . ?
N3 C7 C8 106.9(12) . . ?
C12 C7 C8 112.1(12) . . ?
N3 C7 H7 108.7 . . ?
C12 C7 H7 108.7 . . ?
C8 C7 H7 108.7 . . ?
C7 C8 C9 108.8(16) . . ?
C7 C8 H8A 109.9 . . ?
C9 C8 H8A 109.9 . . ?
C7 C8 H8B 109.9 . . ?
C9 C8 H8B 109.9 . . ?
H8A C8 H8B 108.3 . . ?
C10 C9 C8 111.6(16) . . ?
C10 C9 H9A 109.3 . . ?
C8 C9 H9A 109.3 . . ?
C10 C9 H9B 109.3 . . ?
C8 C9 H9B 109.3 . . ?
H9A C9 H9B 108.0 . . ?
C11 C10 C9 109.8(14) . . ?
C11 C10 H10A 109.7 . . ?
C9 C10 H10A 109.7 . . ?
C11 C10 H10B 109.7 . . ?
C9 C10 H10B 109.7 . . ?
H10A C10 H10B 108.2 . . ?
C10 C11 C12 113.3(17) . . ?
C10 C11 H11A 108.9 . . ?
C12 C11 H11A 108.9 . . ?
C10 C11 H11B 108.9 . . ?
C12 C11 H11B 108.9 . . ?
H11A C11 H11B 107.7 . . ?
N4 C12 C11 110.9(15) . . ?
N4 C12 C7 111.4(11) . . ?
C11 C12 C7 108.7(13) . . ?
N4 C12 H12 108.6 . . ?
C11 C12 H12 108.6 . . ?
C7 C12 H12 108.6 . . ?

_refine_diff_density_max         1.737
_refine_diff_density_min         -2.241
_refine_diff_density_rms         0.232



