# Supplementary Information (SI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2024

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

data_zixuan46
_database_code_depnum_ccdc_archive 'CCDC 2348604'
loop_
_audit_author_name
_audit_author_address
'ZIXUAN ZHANG'
;Hong Kong University of Science and Technology
Hong Kong
;
_audit_update_record             
;
2024-04-16 deposited with the CCDC.	2024-10-30 downloaded from the CCDC.
;
_audit_creation_date             2023-10-06
_audit_creation_method           
;
Olex2 1.5-alpha
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br4 Pb, 2(C8 H11 Br N)'
_chemical_formula_sum            'C16 H22 Br6 N2 Pb'
_chemical_formula_weight         929.00
_chemical_absolute_configuration ad
_chemical_melting_point          ?
# end Validation Reply Form
_chemical_oxdiff_formula         'Pb Br5 N2 C20 H28'
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'
Br Br -0.6763 1.2805 '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'
Pb Pb -4.0753 8.5060 '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           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   8.73840(10)
_cell_length_b                   7.84410(10)
_cell_length_c                   17.9204(2)
_cell_angle_alpha                90
_cell_angle_beta                 97.8460(10)
_cell_angle_gamma                90
_cell_volume                     1216.85(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8231
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      74.4160
_cell_measurement_theta_min      4.9670
_shelx_estimated_absorpt_T_max   0.520
_shelx_estimated_absorpt_T_min   0.082
_exptl_absorpt_coefficient_mu    25.048
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.09491
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.535
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9475
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.513
_diffrn_reflns_theta_min         2.489
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3577
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -93.00 -17.00   1.00    1.50    --  -41.26 -37.00   0.00   76
  2  ω   -119.00  -3.00   1.00    1.50    --  -41.26 -19.00  90.00  116
  3  ω    -48.00  -7.00   1.00    1.50    --  -41.26 125.00-180.00   41
  4  ω     28.00  95.00   1.00    1.50    --   41.26-125.00 -30.00   67
  5  ω     31.00  58.00   1.00    1.50    --   41.26-125.00-180.00   27
  6  ω     16.00  59.00   1.00    1.50    --   41.26  57.00  30.00   43
  7  ω     78.00 105.00   1.00    3.00    --  107.01  61.00  30.00   27
  8  ω     79.00 106.00   1.00    3.00    --  107.01  60.00 -14.72   27
  9  ω    112.00 177.00   1.00    3.00    --  107.01  69.00 -49.34   65
 10  ω     31.00 127.00   1.00    3.00    --  107.01 -77.00-120.00   96
 11  ω     82.00 107.00   1.00    3.00    --  107.01  45.00   0.00   25
 12  ω     34.00 121.00   1.00    3.00    --  107.01 -45.00 -90.00   87
 13  ω     78.00 177.00   1.00    3.00    --  107.01  61.00  60.00   99
 14  ω     58.00 177.00   1.00    3.00    --  107.01  15.00-180.00  119
 15  ω     78.00 109.00   1.00    3.00    --  107.01  61.00 -30.00   31
 16  ω    146.00 172.00   1.00    3.00    --  107.01  61.00   0.00   26
 17  ω     79.00 104.00   1.00    3.00    --  107.01  61.00 -60.00   25
 18  ω     82.00 138.00   1.00    3.00    --  107.01  45.00  60.00   56
 19  ω     81.00 115.00   1.00    3.00    --  107.01  45.00  30.00   34
 20  ω    107.00 156.00   1.00    3.00    --  107.01 111.00 -30.00   49
 21  ω     81.00 108.00   1.00    3.00    --  107.01  45.00 -30.00   27
 22  ω     78.00 104.00   1.00    3.00    --  107.01  61.00   0.00   26
 23  ω     77.00 104.00   1.00    3.00    --  107.01  69.00 -49.34   27
 24  ω     82.00 157.00   1.00    3.00    --  107.01  44.00  43.01   75
;
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0944320000
_diffrn_orient_matrix_UB_12      0.0945593000
_diffrn_orient_matrix_UB_13      -0.0537672000
_diffrn_orient_matrix_UB_21      -0.1452170000
_diffrn_orient_matrix_UB_22      0.0135909000
_diffrn_orient_matrix_UB_23      -0.0589361000
_diffrn_orient_matrix_UB_31      -0.0402632000
_diffrn_orient_matrix_UB_32      0.1717138000
_diffrn_orient_matrix_UB_33      0.0341892000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           0.80
_diffrn_source_power             0.040
_diffrn_source_target            Cu
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_source_voltage           50
_reflns_Friedel_coverage         0.795
_reflns_Friedel_fraction_full    0.960
_reflns_Friedel_fraction_max     0.911
_reflns_number_gt                4621
_reflns_number_total             4738
_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 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_refine_diff_density_max         2.918
_refine_diff_density_min         -2.067
_refine_diff_density_rms         0.332
_refine_ls_abs_structure_details 
;
 Flack x determined using 1975 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.029(12)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         4738
_refine_ls_number_restraints     100
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0476
_refine_ls_restrained_S_all      1.053
_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)+(0.1102P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1329
_refine_ls_wR_factor_ref         0.1340
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 C17, C11, C16, C15, C14, C13, C12, Br12
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Br11, C5, C4, C3, C2, C1, C6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3.a Ternary CH refined with riding coordinates:
 C7(H7), C17(H17)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C6(H6), C12(H12), C14(H14), C15(H15), C16(H16)
3.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), C8(H8A,H8B,H8C), N2(H2A,H2B,H2C), C18(H18A,H18B,H18C)
;
_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 0.25040(4) 0.66908(12) -0.00084(2) 0.01679(18) Uani 1 1 d . . . . .
Br1 Br 0.16529(18) 0.7322(2) -0.16491(8) 0.0238(3) Uani 1 1 d . . . . .
Br2 Br 0.07403(14) 0.33629(18) -0.01795(7) 0.0236(3) Uani 1 1 d . . . . .
Br3 Br 0.32597(16) 0.69218(18) 0.16625(7) 0.0212(3) Uani 1 1 d . . . . .
Br4 Br 0.46126(15) 0.97732(18) 0.00967(7) 0.0261(3) Uani 1 1 d . . . . .
Br11 Br 0.6474(3) 0.2762(2) 0.41482(9) 0.0534(5) Uani 1 1 d . U . . .
N1 N 0.7059(13) 0.6541(18) 0.1523(6) 0.025(2) Uani 1 1 d . . . . .
H1A H 0.7306 0.7035 0.1096 0.030 Uiso 1 1 calc R U . . .
H1B H 0.6014 0.6528 0.1508 0.030 Uiso 1 1 calc R U . . .
H1C H 0.7425 0.5454 0.1557 0.030 Uiso 1 1 calc R U . . .
C1 C 0.6998(16) 0.7057(18) 0.2886(7) 0.026(2) Uani 1 1 d . U . . .
C2 C 0.6306(16) 0.833(2) 0.3264(7) 0.031(2) Uani 1 1 d . U . . .
H2 H 0.6278 0.9475 0.3085 0.038 Uiso 1 1 calc R U . . .
C3 C 0.5664(19) 0.792(2) 0.3898(8) 0.039(3) Uani 1 1 d . U . . .
H3 H 0.5211 0.8794 0.4164 0.047 Uiso 1 1 calc R U . . .
C4 C 0.5666(18) 0.623(2) 0.4162(7) 0.035(2) Uani 1 1 d . U . . .
H4 H 0.5181 0.5939 0.4589 0.042 Uiso 1 1 calc R U . . .
C5 C 0.6387(17) 0.499(2) 0.3786(7) 0.031(2) Uani 1 1 d . U . . .
C6 C 0.7079(18) 0.540(2) 0.3145(7) 0.028(2) Uani 1 1 d . U . . .
H6 H 0.7591 0.4543 0.2896 0.034 Uiso 1 1 calc R U . . .
C7 C 0.7778(17) 0.755(2) 0.2204(7) 0.028(3) Uani 1 1 d . . . . .
H7 H 0.7591 0.8795 0.2099 0.033 Uiso 1 1 calc R U . . .
C8 C 0.9469(17) 0.724(3) 0.2305(9) 0.044(4) Uani 1 1 d . . . . .
H8A H 0.9666 0.6016 0.2366 0.066 Uiso 1 1 calc R U . . .
H8B H 0.9956 0.7846 0.2754 0.066 Uiso 1 1 calc R U . . .
H8C H 0.9901 0.7654 0.1861 0.066 Uiso 1 1 calc R U . . .
Br12 Br 0.1230(2) 0.5160(3) 0.44602(10) 0.0567(5) Uani 1 1 d . U . . .
N2 N 0.1910(13) 0.1020(17) 0.1429(6) 0.024(2) Uani 1 1 d . . . . .
H2A H 0.1978 0.1335 0.0946 0.028 Uiso 1 1 calc R U . . .
H2B H 0.0898 0.0949 0.1496 0.028 Uiso 1 1 calc R U . . .
H2C H 0.2370 -0.0013 0.1523 0.028 Uiso 1 1 calc R U . . .
C11 C 0.2318(14) 0.2006(18) 0.2748(7) 0.023(2) Uani 1 1 d . U . . .
C12 C 0.2011(15) 0.343(2) 0.3170(7) 0.029(2) Uani 1 1 d . U . . .
H12 H 0.2028 0.4541 0.2961 0.035 Uiso 1 1 calc R U . . .
C13 C 0.1679(16) 0.320(2) 0.3896(7) 0.033(2) Uani 1 1 d . U . . .
C14 C 0.1631(16) 0.162(2) 0.4211(7) 0.036(2) Uani 1 1 d . U . . .
H14 H 0.1356 0.1493 0.4703 0.043 Uiso 1 1 calc R U . . .
C15 C 0.199(2) 0.021(2) 0.3806(8) 0.040(3) Uani 1 1 d . U . . .
H15 H 0.1983 -0.0893 0.4028 0.048 Uiso 1 1 calc R U . . .
C16 C 0.2353(18) 0.038(2) 0.3065(8) 0.030(3) Uani 1 1 d . U . . .
H16 H 0.2617 -0.0589 0.2790 0.036 Uiso 1 1 calc R U . . .
C17 C 0.2699(14) 0.231(2) 0.1955(7) 0.023(2) Uani 1 1 d . U . . .
H17 H 0.2297 0.3458 0.1786 0.027 Uiso 1 1 calc R U . . .
C18 C 0.4423(14) 0.2276(18) 0.1908(7) 0.026(3) Uani 1 1 d . . . . .
H18A H 0.4789 0.1094 0.1933 0.039 Uiso 1 1 calc R U . . .
H18B H 0.4972 0.2924 0.2330 0.039 Uiso 1 1 calc R U . . .
H18C H 0.4619 0.2789 0.1431 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
Pb1 Br1 2.9743(15) . ?
Pb1 Br2 3.0257(16) . ?
Pb1 Br2 3.1830(13) 2 ?
Pb1 Br3 2.9825(13) . ?
Pb1 Br4 2.9572(15) 2_645 ?
Pb1 Br4 3.0301(16) . ?
Br2 Pb1 3.1830(13) 2_545 ?
Br4 Pb1 2.9572(15) 2_655 ?
Br11 C5 1.865(16) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 H1C 0.9100 . ?
N1 C7 1.519(17) . ?
C1 C2 1.39(2) . ?
C1 C6 1.38(2) . ?
C1 C7 1.529(17) . ?
C2 H2 0.9500 . ?
C2 C3 1.372(19) . ?
C3 H3 0.9500 . ?
C3 C4 1.41(2) . ?
C4 H4 0.9500 . ?
C4 C5 1.38(2) . ?
C5 C6 1.404(18) . ?
C6 H6 0.9500 . ?
C7 H7 1.0000 . ?
C7 C8 1.48(2) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
Br12 C13 1.913(15) . ?
N2 H2A 0.9100 . ?
N2 H2B 0.9100 . ?
N2 H2C 0.9100 . ?
N2 C17 1.485(17) . ?
C11 C12 1.394(18) . ?
C11 C16 1.40(2) . ?
C11 C17 1.523(17) . ?
C12 H12 0.9500 . ?
C12 C13 1.384(18) . ?
C13 C14 1.36(2) . ?
C14 H14 0.9500 . ?
C14 C15 1.38(2) . ?
C15 H15 0.9500 . ?
C15 C16 1.416(18) . ?
C16 H16 0.9500 . ?
C17 H17 1.0000 . ?
C17 C18 1.520(17) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 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
Br1 Pb1 Br2 85.98(4) . 2 ?
Br1 Pb1 Br2 89.33(4) . . ?
Br1 Pb1 Br3 166.80(5) . . ?
Br1 Pb1 Br4 89.80(4) . . ?
Br2 Pb1 Br2 85.268(18) . 2 ?
Br2 Pb1 Br4 172.63(4) . . ?
Br3 Pb1 Br2 101.19(4) . . ?
Br3 Pb1 Br2 86.97(4) . 2 ?
Br3 Pb1 Br4 80.78(4) . . ?
Br4 Pb1 Br1 97.57(4) 2_645 . ?
Br4 Pb1 Br2 101.97(5) . 2 ?
Br4 Pb1 Br2 173.19(5) 2_645 2 ?
Br4 Pb1 Br2 88.95(5) 2_645 . ?
Br4 Pb1 Br3 90.64(4) 2_645 . ?
Br4 Pb1 Br4 83.909(14) 2_645 . ?
Pb1 Br2 Pb1 142.51(5) . 2_545 ?
Pb1 Br4 Pb1 156.62(6) 2_655 . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C7 N1 H1A 109.5 . . ?
C7 N1 H1B 109.5 . . ?
C7 N1 H1C 109.5 . . ?
C2 C1 C7 118.4(13) . . ?
C6 C1 C2 121.3(13) . . ?
C6 C1 C7 120.1(13) . . ?
C1 C2 H2 120.4 . . ?
C3 C2 C1 119.2(15) . . ?
C3 C2 H2 120.4 . . ?
C2 C3 H3 119.4 . . ?
C2 C3 C4 121.1(15) . . ?
C4 C3 H3 119.4 . . ?
C3 C4 H4 120.8 . . ?
C5 C4 C3 118.4(13) . . ?
C5 C4 H4 120.8 . . ?
C4 C5 Br11 119.1(10) . . ?
C4 C5 C6 121.3(15) . . ?
C6 C5 Br11 119.6(12) . . ?
C1 C6 C5 118.6(14) . . ?
C1 C6 H6 120.7 . . ?
C5 C6 H6 120.7 . . ?
N1 C7 C1 109.1(11) . . ?
N1 C7 H7 108.6 . . ?
C1 C7 H7 108.6 . . ?
C8 C7 N1 107.9(12) . . ?
C8 C7 C1 113.9(12) . . ?
C8 C7 H7 108.6 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
H2A N2 H2B 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
C17 N2 H2A 109.5 . . ?
C17 N2 H2B 109.5 . . ?
C17 N2 H2C 109.5 . . ?
C12 C11 C16 120.5(12) . . ?
C12 C11 C17 117.7(13) . . ?
C16 C11 C17 121.7(12) . . ?
C11 C12 H12 120.5 . . ?
C13 C12 C11 119.0(15) . . ?
C13 C12 H12 120.5 . . ?
C12 C13 Br12 118.3(13) . . ?
C14 C13 Br12 119.5(10) . . ?
C14 C13 C12 122.2(14) . . ?
C13 C14 H14 120.4 . . ?
C13 C14 C15 119.2(13) . . ?
C15 C14 H14 120.4 . . ?
C14 C15 H15 119.6 . . ?
C14 C15 C16 120.8(16) . . ?
C16 C15 H15 119.6 . . ?
C11 C16 C15 118.2(14) . . ?
C11 C16 H16 120.9 . . ?
C15 C16 H16 120.9 . . ?
N2 C17 C11 110.2(11) . . ?
N2 C17 H17 108.0 . . ?
N2 C17 C18 109.4(11) . . ?
C11 C17 H17 108.0 . . ?
C18 C17 C11 113.2(10) . . ?
C18 C17 H17 108.0 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Br11 C5 C6 C1 179.9(11) . . . . ?
C1 C2 C3 C4 -1(2) . . . . ?
C2 C1 C6 C5 3(2) . . . . ?
C2 C1 C7 N1 -122.9(14) . . . . ?
C2 C1 C7 C8 116.4(16) . . . . ?
C2 C3 C4 C5 3(2) . . . . ?
C3 C4 C5 Br11 177.5(11) . . . . ?
C3 C4 C5 C6 -1(2) . . . . ?
C4 C5 C6 C1 -1(2) . . . . ?
C6 C1 C2 C3 -1(2) . . . . ?
C6 C1 C7 N1 61.4(17) . . . . ?
C6 C1 C7 C8 -59.2(19) . . . . ?
C7 C1 C2 C3 -176.9(13) . . . . ?
C7 C1 C6 C5 178.2(12) . . . . ?
Br12 C13 C14 C15 -178.8(12) . . . . ?
C11 C12 C13 Br12 -179.1(10) . . . . ?
C11 C12 C13 C14 -1(2) . . . . ?
C12 C11 C16 C15 3(2) . . . . ?
C12 C11 C17 N2 -138.3(12) . . . . ?
C12 C11 C17 C18 98.9(15) . . . . ?
C12 C13 C14 C15 3(2) . . . . ?
C13 C14 C15 C16 -2(2) . . . . ?
C14 C15 C16 C11 -1(2) . . . . ?
C16 C11 C12 C13 -2.6(19) . . . . ?
C16 C11 C17 N2 45.1(16) . . . . ?
C16 C11 C17 C18 -77.7(17) . . . . ?
C17 C11 C12 C13 -179.2(11) . . . . ?
C17 C11 C16 C15 179.9(13) . . . . ?


_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 5.470
_oxdiff_exptl_absorpt_empirical_full_min 0.527
# start Validation Reply Form
_vrf_PLAT971_zixuan46            
;
PROBLEM: Check Calcd Resid. Dens. 0.74Ang From Pb1 2.87 eA-3
RESPONSE: The big residual density peaks (and holes) located closely to the 
heaviest atom(s) could not be a real atom.  It is generally known as the 
'absorption problem' (especial with Cu-Ka we used here) and little can be 
done after the absorption correction applied. 
;
####################################################################### 
# 
# 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_3-cl-mba-pbbr
_database_code_depnum_ccdc_archive 'CCDC 2348605'
loop_
_audit_author_name
_audit_author_address
'ZIXUAN ZHANG'
;Hong Kong University of Science and Technology
Hong Kong
;
_audit_update_record             
;
2024-04-16 deposited with the CCDC.	2024-10-30 downloaded from the CCDC.
;
_audit_creation_date             2024-03-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br4 Pb, 2(C8 H11 Cl N)'
_chemical_formula_sum            'C16 H22 Br4 Cl2 N2 Pb'
_chemical_formula_weight         840.08
_chemical_absolute_configuration R
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Pb I Cl C N'
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'
Cl Cl 0.1484 0.1585 '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           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   8.7598(2)
_cell_length_b                   7.7798(2)
_cell_length_c                   17.5050(4)
_cell_angle_alpha                90
_cell_angle_beta                 97.984(2)
_cell_angle_gamma                90
_cell_volume                     1181.39(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5213
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.6200
_cell_measurement_theta_min      2.3390
_shelx_estimated_absorpt_T_max   0.438
_shelx_estimated_absorpt_T_min   0.305
_exptl_absorpt_coefficient_mu    14.135
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36143
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.43.90 (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.362
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_av_unetI/netI     0.0469
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            7306
_diffrn_reflns_point_group_measured_fraction_full 0.934
_diffrn_reflns_point_group_measured_fraction_max 0.926
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.731
_diffrn_reflns_theta_min         2.348
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3577
_diffrn_detector_type            Atlas
_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    -40.00  49.00   1.00    2.50    --   15.85 -77.00-120.00   89
  2  ω    -40.00  50.00   1.00    2.50    --   15.85 -77.00 120.00   90
  3  ω    -41.00  50.00   1.00    2.50    --   15.85 -77.00   0.00   91
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0112390000
_diffrn_orient_matrix_UB_12      -0.0078378000
_diffrn_orient_matrix_UB_13      0.0392060000
_diffrn_orient_matrix_UB_21      0.0255938000
_diffrn_orient_matrix_UB_22      0.0858594000
_diffrn_orient_matrix_UB_23      0.0068711000
_diffrn_orient_matrix_UB_31      -0.0768147000
_diffrn_orient_matrix_UB_32      0.0297264000
_diffrn_orient_matrix_UB_33      -0.0094563000
_diffrn_oxdiff_digest_frames     
;
01a077a30a747393495c3aa531c2a1f46e00284d2b5
;
_diffrn_oxdiff_digest_hkl        
;
01ba0dc6263eeef0982004e0b2d5abaac0ed6e
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.724
_reflns_Friedel_fraction_full    0.858
_reflns_Friedel_fraction_max     0.842
_reflns_number_gt                4383
_reflns_number_total             4643
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_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 1.171.43.90 (Rigaku OD, 2023)'
_computing_data_collection       
'CrysAlisPro system (CCD 43.90 (release 15-09-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.942
_refine_diff_density_min         -1.389
_refine_diff_density_rms         0.182
_refine_ls_abs_structure_details 
;
 Flack x determined using 1708 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.040(7)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         4643
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0307
_refine_ls_restrained_S_all      1.032
_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)+(0.0325P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0673
_refine_ls_wR_factor_ref         0.0691
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C00B) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3.a Ternary CH refined with riding coordinates:
 C00G(H00S), C00H(H00H)
3.b Aromatic/amide H refined with riding coordinates:
 C00C(H00Q), C00D(H00R), C00F(H00F), C00J(H00T), C00L(H00U), C00O(H00O),
 C00P(H00P), C1(H1)
3.c Idealised Me refined as rotating group:
 N008(H00A,H00B,H00C), N009(H00I,H00J,H00K), C00B(H00L,H00M,H00N), C00K(H00D,
 H00E,H00G)
;
_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 0.74903(3) 0.52345(6) 0.50036(2) 0.00767(9) Uani 1 1 d . . . . .
Br02 Br 0.92573(10) 0.18840(13) 0.51951(5) 0.0117(2) Uani 1 1 d . . . . .
Br03 Br 0.46052(10) 0.33366(13) 0.50918(5) 0.0132(2) Uani 1 1 d . . . . .
Br04 Br 0.83375(11) 0.58574(12) 0.66815(6) 0.0119(2) Uani 1 1 d . . . . .
Br05 Br 0.67210(10) 0.54976(12) 0.32906(5) 0.0102(2) Uani 1 1 d . . . . .
Cl06 Cl 0.3634(4) 0.1292(4) 0.08550(16) 0.0314(7) Uani 1 1 d . . . . .
Cl07 Cl 0.8654(3) 0.3734(4) 0.04957(16) 0.0300(7) Uani 1 1 d . . . . .
N008 N 0.2935(8) 0.5135(11) 0.3434(4) 0.0137(17) Uani 1 1 d . . . . .
H00A H 0.270520 0.399686 0.338146 0.016 Uiso 1 1 calc GR . . . .
H00B H 0.254924 0.555914 0.385290 0.016 Uiso 1 1 calc GR . . . .
H00C H 0.397586 0.527616 0.349928 0.016 Uiso 1 1 calc GR . . . .
N009 N 0.8115(8) -0.0430(10) 0.3542(5) 0.0112(17) Uani 1 1 d . . . . .
H00I H 0.774774 -0.149252 0.339783 0.013 Uiso 1 1 calc GR . . . .
H00J H 0.793637 -0.020709 0.403186 0.013 Uiso 1 1 calc GR . . . .
H00K H 0.914715 -0.039244 0.352117 0.013 Uiso 1 1 calc GR . . . .
C00A C 0.7695(10) 0.0640(11) 0.2194(5) 0.010(2) Uani 1 1 d . . . . .
C00B C 0.5600(11) 0.0836(12) 0.3060(6) 0.015(2) Uani 1 1 d . U . . .
H00L H 0.518519 -0.028729 0.288308 0.023 Uiso 1 1 calc GR . . . .
H00M H 0.507051 0.174178 0.273604 0.023 Uiso 1 1 calc GR . . . .
H00N H 0.543883 0.101489 0.359717 0.023 Uiso 1 1 calc GR . . . .
C00C C 0.7958(10) 0.2064(14) 0.1762(6) 0.015(2) Uani 1 1 d . . . . .
H00Q H 0.789271 0.317819 0.197696 0.017 Uiso 1 1 calc R . . . .
C00D C 0.7729(11) -0.0965(13) 0.1849(6) 0.014(2) Uani 1 1 d . . . . .
H00R H 0.749158 -0.196060 0.212384 0.017 Uiso 1 1 calc R . . . .
C00E C 0.2999(10) 0.5547(12) 0.2043(5) 0.010(2) Uani 1 1 d . . . . .
C00F C 0.2943(11) 0.3851(13) 0.1784(6) 0.015(2) Uani 1 1 d . . . . .
H00F H 0.237962 0.300728 0.201999 0.018 Uiso 1 1 calc R . . . .
C00G C 0.7314(11) 0.0896(13) 0.3004(5) 0.012(2) Uani 1 1 d . . . . .
H00S H 0.770740 0.205205 0.318657 0.015 Uiso 1 1 calc R . . . .
C00H C 0.2222(11) 0.6094(14) 0.2715(6) 0.016(2) Uani 1 1 d . . . . .
H00H H 0.238216 0.735561 0.280000 0.019 Uiso 1 1 calc R . . . .
C00I C 0.8313(11) 0.1896(14) 0.1024(6) 0.016(2) Uani 1 1 d . . . . .
C00J C 0.8411(11) 0.0292(16) 0.0689(6) 0.021(2) Uani 1 1 d . . . . .
H00T H 0.868316 0.018080 0.018480 0.025 Uiso 1 1 calc R . . . .
C00K C 0.0504(11) 0.5716(13) 0.2603(6) 0.024(3) Uani 1 1 d . . . . .
H00D H 0.033236 0.450144 0.246962 0.036 Uiso 1 1 calc GR . . . .
H00E H -0.001410 0.643561 0.218596 0.036 Uiso 1 1 calc GR . . . .
H00G H 0.008453 0.596770 0.308172 0.036 Uiso 1 1 calc GR . . . .
C00L C 0.8104(11) -0.1137(15) 0.1107(6) 0.021(2) Uani 1 1 d . . . . .
H00U H 0.814896 -0.224807 0.088615 0.025 Uiso 1 1 calc R . . . .
C00M C 0.3721(11) 0.3422(14) 0.1178(5) 0.016(2) Uani 1 1 d . . . . .
C00O C 0.4497(11) 0.4615(15) 0.0799(6) 0.023(3) Uani 1 1 d . . . . .
H00O H 0.500950 0.428244 0.037794 0.027 Uiso 1 1 calc R . . . .
C00P C 0.3776(11) 0.6770(14) 0.1661(5) 0.018(2) Uani 1 1 d . . . . .
H00P H 0.379719 0.793255 0.182818 0.022 Uiso 1 1 calc R . . . .
C1 C 0.4517(12) 0.6321(15) 0.1042(6) 0.024(3) Uani 1 1 d . . . . .
H1 H 0.503643 0.716983 0.078471 0.029 Uiso 1 1 calc R . . . .


_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 3.0263(11) . ?
Pb01 Br02 3.1875(10) 2_756 ?
Pb01 Br03 2.9495(10) . ?
Pb01 Br03 3.0227(11) 2_656 ?
Pb01 Br04 2.9676(10) . ?
Pb01 Br05 2.9878(10) . ?
Cl06 C00M 1.749(11) . ?
Cl07 C00I 1.751(11) . ?
N008 C00H 1.521(12) . ?
N009 C00G 1.503(12) . ?
C00A C00C 1.379(13) . ?
C00A C00D 1.390(13) . ?
C00A C00G 1.514(13) . ?
C00B C00G 1.519(13) . ?
C00C C00I 1.376(14) . ?
C00D C00L 1.389(14) . ?
C00E C00F 1.394(14) . ?
C00E C00H 1.501(13) . ?
C00E C00P 1.394(13) . ?
C00F C00M 1.379(13) . ?
C00H C00K 1.519(13) . ?
C00I C00J 1.387(15) . ?
C00J C00L 1.377(15) . ?
C00M C00O 1.375(14) . ?
C00O C1 1.394(15) . ?
C00P C1 1.382(15) . ?

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 84.704(14) . 2_756 ?
Br03 Pb01 Br02 102.57(3) 2_656 2_756 ?
Br03 Pb01 Br02 89.53(3) . . ?
Br03 Pb01 Br02 172.37(3) 2_656 . ?
Br03 Pb01 Br02 173.03(3) . 2_756 ?
Br03 Pb01 Br03 83.362(11) . 2_656 ?
Br03 Pb01 Br04 97.37(3) . . ?
Br03 Pb01 Br05 90.65(3) . . ?
Br04 Pb01 Br02 88.70(3) . . ?
Br04 Pb01 Br02 86.44(3) . 2_756 ?
Br04 Pb01 Br03 89.47(3) . 2_656 ?
Br04 Pb01 Br05 166.58(3) . . ?
Br05 Pb01 Br02 102.17(3) . . ?
Br05 Pb01 Br02 86.75(3) . 2_756 ?
Br05 Pb01 Br03 80.75(3) . 2_656 ?
Pb01 Br02 Pb01 141.80(4) . 2_746 ?
Pb01 Br03 Pb01 156.20(4) . 2_646 ?
C00C C00A C00D 117.9(9) . . ?
C00C C00A C00G 118.9(8) . . ?
C00D C00A C00G 123.1(8) . . ?
C00I C00C C00A 121.0(10) . . ?
C00L C00D C00A 121.0(9) . . ?
C00F C00E C00H 121.6(9) . . ?
C00P C00E C00F 119.2(9) . . ?
C00P C00E C00H 119.2(9) . . ?
C00M C00F C00E 118.7(9) . . ?
N009 C00G C00A 110.6(8) . . ?
N009 C00G C00B 108.6(8) . . ?
C00A C00G C00B 113.9(8) . . ?
C00E C00H N008 109.4(8) . . ?
C00E C00H C00K 113.2(8) . . ?
C00K C00H N008 107.3(8) . . ?
C00C C00I Cl07 119.7(9) . . ?
C00C C00I C00J 121.2(10) . . ?
C00J C00I Cl07 119.1(8) . . ?
C00L C00J C00I 118.3(9) . . ?
C00J C00L C00D 120.5(10) . . ?
C00F C00M Cl06 118.3(8) . . ?
C00O C00M Cl06 119.1(8) . . ?
C00O C00M C00F 122.6(10) . . ?
C00M C00O C1 118.8(10) . . ?
C1 C00P C00E 121.1(10) . . ?
C00P C1 C00O 119.5(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 1.727
_oxdiff_exptl_absorpt_empirical_full_min 0.734
####################################################################### 
# 
# 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_pbi-3-cl-mba
_database_code_depnum_ccdc_archive 'CCDC 2348609'
loop_
_audit_author_name
_audit_author_address
'ZIXUAN ZHANG'
;Hong Kong University of Science and Technology
Hong Kong
;
_audit_update_record             
;
2024-04-16 deposited with the CCDC.	2024-10-30 downloaded from the CCDC.
;
_audit_creation_date             2024-03-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'I4 Pb, 2(C8 H11 Cl N)'
_chemical_formula_sum            'C16 H22 Cl2 I4 N2 Pb'
_chemical_formula_weight         1028.04
_chemical_absolute_configuration R
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C N Pb I Cl'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   9.1762(2)
_cell_length_b                   8.18250(10)
_cell_length_c                   17.4483(3)
_cell_angle_alpha                90
_cell_angle_beta                 98.856(2)
_cell_angle_gamma                90
_cell_volume                     1294.47(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6261
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      29.7670
_cell_measurement_theta_min      2.3670
_shelx_estimated_absorpt_T_max   0.724
_shelx_estimated_absorpt_T_min   0.500
_exptl_absorpt_coefficient_mu    11.497
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62291
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.43.90 (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.638
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.07
_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  0.0250
_diffrn_reflns_av_unetI/netI     0.0397
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            8228
_diffrn_reflns_point_group_measured_fraction_full 0.865
_diffrn_reflns_point_group_measured_fraction_max 0.843
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.729
_diffrn_reflns_theta_min         2.363
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3577
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_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    -85.00  10.00   1.00    5.00    --  -15.31 -57.00-120.00   95
  2  ω    -36.00  48.00   1.00    5.00    --   15.85 -77.00  30.00   84
  3  ω    -10.00  89.00   1.00    5.00    --   15.85  57.00-180.00   99
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0699634000
_diffrn_orient_matrix_UB_12      0.0386978000
_diffrn_orient_matrix_UB_13      0.0071183000
_diffrn_orient_matrix_UB_21      -0.0069495000
_diffrn_orient_matrix_UB_22      0.0085217000
_diffrn_orient_matrix_UB_23      0.0397196000
_diffrn_orient_matrix_UB_31      0.0342997000
_diffrn_orient_matrix_UB_32      -0.0771316000
_diffrn_orient_matrix_UB_33      0.0079498000
_diffrn_oxdiff_digest_frames     
;
01e4d7bfd09560c9b472123072d07cd3320002831c0
;
_diffrn_oxdiff_digest_hkl        
;
012b75d3e852b110da97cc797b591a2bfa173e
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.575
_reflns_Friedel_fraction_full    0.710
_reflns_Friedel_fraction_max     0.664
_reflns_number_gt                4462
_reflns_number_total             4650
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_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 1.171.43.90 (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.713
_refine_diff_density_min         -1.229
_refine_diff_density_rms         0.183
_refine_ls_abs_structure_details 
;
 Flack x determined using 1563 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.020(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         4650
_refine_ls_number_restraints     31
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0227
_refine_ls_restrained_S_all      0.996
_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)+(0.0171P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0465
_refine_ls_wR_factor_ref         0.0473
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C00D) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C00I) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C00M) \\sim Ueq, Uanis(C00J) \\sim Ueq, Uanis(C00K) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
3.a Ternary CH refined with riding coordinates:
 C00A(H00M), C00F(H00F)
3.b Aromatic/amide H refined with riding coordinates:
 C00D(H00R), C00E(H00S), C00J(H00J), C00L(H00L), C00M(H00T), C00N(H00U),
 C00P(H00P), C1(H1)
3.c Idealised Me refined as rotating group:
 N008(H00A,H00B,H00C), N009(H00H,H00I,H00K), C00C(H00N,H00O,H00Q), C00H(H00D,
 H00E,H00G)
;
_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 -0.25039(3) 0.75658(4) 0.00081(2) 0.00977(7) Uani 1 1 d . . . . .
I002 I -0.07153(6) 0.41776(6) 0.02126(3) 0.01192(12) Uani 1 1 d . . . . .
I003 I -0.54968(6) 0.57522(6) 0.00963(3) 0.01405(12) Uani 1 1 d . . . . .
I004 I -0.32764(6) 0.76894(6) -0.18278(3) 0.01176(12) Uani 1 1 d . . . . .
I005 I -0.16682(6) 0.81018(6) 0.18280(3) 0.01348(13) Uani 1 1 d . . . . .
Cl06 Cl 0.6249(3) 0.8716(3) 0.41776(13) 0.0336(6) Uani 1 1 d . . . . .
Cl07 Cl 0.1385(3) 1.0865(3) 0.45991(13) 0.0316(6) Uani 1 1 d . . . . .
N008 N 0.7184(7) 1.2489(9) 0.1706(4) 0.0151(15) Uani 1 1 d . . . . .
H00A H 0.759560 1.287994 0.130049 0.018 Uiso 1 1 calc GR . . . .
H00B H 0.619216 1.266045 0.161454 0.018 Uiso 1 1 calc GR . . . .
H00C H 0.736735 1.139922 0.176065 0.018 Uiso 1 1 calc GR . . . .
N009 N 0.1934(7) 0.6827(8) 0.1571(4) 0.0123(15) Uani 1 1 d . . . . .
H00H H 0.212021 0.702301 0.108195 0.015 Uiso 1 1 calc GR . . . .
H00I H 0.094406 0.686166 0.157502 0.015 Uiso 1 1 calc GR . . . .
H00K H 0.228472 0.582130 0.172808 0.015 Uiso 1 1 calc GR . . . .
C00A C 0.2687(9) 0.8113(10) 0.2116(4) 0.0135(18) Uani 1 1 d . . . . .
H00M H 0.231039 0.920713 0.192229 0.016 Uiso 1 1 calc R . . . .
C00B C 0.2295(9) 0.7875(8) 0.2926(4) 0.0105(17) Uani 1 1 d . . . . .
C00C C 0.4319(9) 0.8056(10) 0.2085(5) 0.018(2) Uani 1 1 d . . . . .
H00N H 0.470329 0.697071 0.224477 0.027 Uiso 1 1 calc GR . . . .
H00O H 0.482455 0.888282 0.243677 0.027 Uiso 1 1 calc GR . . . .
H00Q H 0.449129 0.827895 0.155478 0.027 Uiso 1 1 calc GR . . . .
C00D C 0.2045(9) 0.9262(11) 0.3341(4) 0.0150(17) Uani 1 1 d . U . . .
H00R H 0.211137 1.031281 0.311709 0.018 Uiso 1 1 calc R . . . .
C00E C 0.2235(9) 0.6356(10) 0.3269(4) 0.0145(18) Uani 1 1 d . . . . .
H00S H 0.243786 0.540277 0.299309 0.017 Uiso 1 1 calc R . . . .
C00F C 0.7841(10) 1.3367(11) 0.2441(5) 0.0192(19) Uani 1 1 d . . . . .
H00F H 0.770091 1.456888 0.235689 0.023 Uiso 1 1 calc R . . . .
C00G C 0.7024(9) 1.2848(9) 0.3094(5) 0.0152(18) Uani 1 1 d . . . . .
C00H C 0.9475(10) 1.3012(11) 0.2599(5) 0.027(2) Uani 1 1 d . . . . .
H00D H 0.963056 1.183747 0.268774 0.041 Uiso 1 1 calc GR . . . .
H00E H 0.992510 1.361717 0.305978 0.041 Uiso 1 1 calc GR . . . .
H00G H 0.993082 1.334962 0.215168 0.041 Uiso 1 1 calc GR . . . .
C00I C 0.1700(9) 0.9119(11) 0.4078(5) 0.0187(18) Uani 1 1 d . U . . .
C00J C 0.7031(10) 1.1211(10) 0.3328(5) 0.0173(19) Uani 1 1 d . U . . .
H00J H 0.759480 1.042576 0.309894 0.021 Uiso 1 1 calc R . . . .
C00K C 0.6220(9) 1.0748(10) 0.3889(5) 0.0187(19) Uani 1 1 d . U . . .
C00L C 0.6230(9) 1.3978(11) 0.3451(4) 0.0182(18) Uani 1 1 d . . . . .
H00L H 0.624931 1.509820 0.330893 0.022 Uiso 1 1 calc R . . . .
C00M C 0.1603(10) 0.7591(11) 0.4422(5) 0.0216(19) Uani 1 1 d . U . . .
H00T H 0.135005 0.750407 0.492800 0.026 Uiso 1 1 calc R . . . .
C00N C 0.1880(10) 0.6211(11) 0.4015(5) 0.023(2) Uani 1 1 d . . . . .
H00U H 0.182944 0.516232 0.424286 0.027 Uiso 1 1 calc R . . . .
C00P C 0.5388(10) 1.1863(12) 0.4234(5) 0.025(2) Uani 1 1 d . . . . .
H00P H 0.481690 1.151872 0.461488 0.030 Uiso 1 1 calc R . . . .
C1 C 0.5407(10) 1.3492(11) 0.4014(5) 0.024(2) Uani 1 1 d . . . . .
H1 H 0.485336 1.427588 0.424899 0.029 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb01 I002 3.2135(6) . ?
Pb01 I002 3.3113(6) 2 ?
Pb01 I003 3.1462(6) . ?
Pb01 I003 3.1771(6) 2_455 ?
Pb01 I004 3.1741(6) . ?
Pb01 I005 3.1804(6) . ?
Cl06 C00K 1.737(9) . ?
Cl07 C00I 1.741(9) . ?
N008 C00F 1.512(10) . ?
N009 C00A 1.513(9) . ?
C00A C00B 1.524(10) . ?
C00A C00C 1.507(11) . ?
C00B C00D 1.384(11) . ?
C00B C00E 1.384(10) . ?
C00D C00I 1.376(10) . ?
C00E C00N 1.395(11) . ?
C00F C00G 1.519(11) . ?
C00F C00H 1.511(12) . ?
C00G C00J 1.400(11) . ?
C00G C00L 1.383(11) . ?
C00I C00M 1.395(12) . ?
C00J C00K 1.371(10) . ?
C00K C00P 1.385(12) . ?
C00L C1 1.386(11) . ?
C00M C00N 1.378(12) . ?
C00P C1 1.389(13) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I002 Pb01 I002 84.665(9) . 2 ?
I003 Pb01 I002 100.609(16) 2_455 2 ?
I003 Pb01 I002 91.282(16) . . ?
I003 Pb01 I002 174.206(15) 2_455 . ?
I003 Pb01 I002 174.073(17) . 2 ?
I003 Pb01 I003 83.638(8) . 2_455 ?
I003 Pb01 I004 90.196(16) . . ?
I003 Pb01 I005 89.564(15) 2_455 . ?
I003 Pb01 I005 95.410(15) . . ?
I004 Pb01 I002 86.249(14) . 2 ?
I004 Pb01 I002 99.815(15) . . ?
I004 Pb01 I003 83.035(15) . 2_455 ?
I004 Pb01 I005 170.179(17) . . ?
I005 Pb01 I002 88.141(15) . . ?
I005 Pb01 I002 88.792(15) . 2 ?
Pb01 I002 Pb01 141.282(19) . 2_545 ?
Pb01 I003 Pb01 152.25(2) . 2_445 ?
N009 C00A C00B 110.1(6) . . ?
C00C C00A N009 108.5(6) . . ?
C00C C00A C00B 114.0(7) . . ?
C00D C00B C00A 117.5(6) . . ?
C00E C00B C00A 123.1(7) . . ?
C00E C00B C00D 119.4(7) . . ?
C00I C00D C00B 119.9(8) . . ?
C00B C00E C00N 120.6(8) . . ?
N008 C00F C00G 109.0(7) . . ?
C00H C00F N008 108.6(7) . . ?
C00H C00F C00G 113.6(7) . . ?
C00J C00G C00F 120.3(7) . . ?
C00L C00G C00F 120.4(7) . . ?
C00L C00G C00J 119.3(8) . . ?
C00D C00I Cl07 119.9(7) . . ?
C00D C00I C00M 121.1(8) . . ?
C00M C00I Cl07 119.0(6) . . ?
C00K C00J C00G 119.5(8) . . ?
C00J C00K Cl06 119.1(6) . . ?
C00J C00K C00P 121.7(8) . . ?
C00P C00K Cl06 119.2(6) . . ?
C00G C00L C1 120.6(8) . . ?
C00N C00M C00I 119.0(7) . . ?
C00M C00N C00E 119.9(8) . . ?
C00K C00P C1 118.7(8) . . ?
C00L C1 C00P 120.2(8) . . ?

_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 1.361
_oxdiff_exptl_absorpt_empirical_full_min 0.793
####################################################################### 
# 
# 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_pbbr-4-brmba
_database_code_depnum_ccdc_archive 'CCDC 2348607'
loop_
_audit_author_name
_audit_author_address
'ZIXUAN ZHANG'
;Hong Kong University of Science and Technology
Hong Kong
;
_audit_update_record             
;
2024-04-16 deposited with the CCDC.	2024-10-30 downloaded from the CCDC.
;
_audit_creation_date             2024-03-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br8 Pb2, 4(C8 H11 Br N), 2(H2 O)'
_chemical_formula_sum            'C32 H48 Br12 N4 O2 Pb2'
_chemical_formula_weight         1894.04
_chemical_absolute_configuration R
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Pb Br C N'
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      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   7.8357(2)
_cell_length_b                   35.9831(11)
_cell_length_c                   8.8981(2)
_cell_angle_alpha                90
_cell_angle_beta                 90.903(2)
_cell_angle_gamma                90
_cell_volume                     2508.53(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9632
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      29.7120
_cell_measurement_theta_min      2.3550
_shelx_estimated_absorpt_T_max   0.641
_shelx_estimated_absorpt_T_min   0.168
_exptl_absorpt_coefficient_mu    16.292
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21466
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.43.90 (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.508
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_unetI/netI     0.0623
_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       -8
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            14228
_diffrn_reflns_point_group_measured_fraction_full 0.867
_diffrn_reflns_point_group_measured_fraction_max 0.867
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.348
_diffrn_reflns_theta_min         2.289
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3577
_diffrn_detector_type            Atlas
_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    -86.00   8.50   0.75   12.00    --  -15.46 -57.00  60.00  126
  2  ω     -9.00  88.50   0.75   12.00    --   15.85  57.00   0.00  130
  3  ω    -35.00  51.25   0.75   12.00    --   15.85 -77.00-150.00  115
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0007341000
_diffrn_orient_matrix_UB_12      -0.0182299000
_diffrn_orient_matrix_UB_13      0.0302791000
_diffrn_orient_matrix_UB_21      -0.0408061000
_diffrn_orient_matrix_UB_22      0.0066485000
_diffrn_orient_matrix_UB_23      0.0652803000
_diffrn_orient_matrix_UB_31      -0.0808279000
_diffrn_orient_matrix_UB_32      -0.0035097000
_diffrn_orient_matrix_UB_33      -0.0342211000
_diffrn_oxdiff_digest_frames     
;
01f82cf9bd4f5debbdca55ef6f06e4812d000276603
;
_diffrn_oxdiff_digest_hkl        
;
0135eb38af3f0b071d0768ab3aae2cd1e9fa16
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.705
_reflns_Friedel_fraction_full    0.731
_reflns_Friedel_fraction_max     0.729
_reflns_number_gt                7556
_reflns_number_total             7980
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_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 1.171.43.90 (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         3.143
_refine_diff_density_min         -2.295
_refine_diff_density_rms         0.328
_refine_ls_abs_structure_details 
;
 Flack x determined using 2733 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.023(10)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     483
_refine_ls_number_reflns         7980
_refine_ls_number_restraints     219
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0508
_refine_ls_restrained_S_all      1.086
_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)+(0.0583P)²+30.7291P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1222
_refine_ls_wR_factor_ref         0.1248
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 H1B-H00R
 2.1 with sigma of 0.01
 H1A-H00B
 2.1 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C01E) \\sim Ueq, Uanis(C00I) \\sim Ueq, Uanis(C00L) \\sim Ueq,
Uanis(N00K) \\sim Ueq, Uanis(N00J) \\sim Ueq, Uanis(C00O) \\sim Ueq,
Uanis(N00M) \\sim Ueq, Uanis(C00U) \\sim Ueq, Uanis(C019) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
Uanis(C00N) \\sim Ueq, Uanis(C017) \\sim Ueq, Uanis(C00V) \\sim Ueq,
Uanis(C00W) \\sim Ueq, Uanis(C012) \\sim Ueq, Uanis(C01A) \\sim Ueq,
Uanis(C01F) \\sim Ueq, Uanis(C00R) \\sim Ueq, Uanis(C00Q) \\sim Ueq,
Uanis(C00S) \\sim Ueq, Uanis(C00X) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C00Y)
\\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C01C) \\sim Ueq, Uanis(C019) \\sim Ueq,
Uanis(C018) \\sim Ueq, Uanis(C00U) \\sim Ueq, Uanis(C010) \\sim Ueq,
Uanis(N00M) \\sim Ueq, Uanis(C00O) \\sim Ueq, Uanis(C00P) \\sim Ueq,
Uanis(N00J) \\sim Ueq, Uanis(N00K) \\sim Ueq, Uanis(C00L) \\sim Ueq,
Uanis(C00I) \\sim Ueq, Uanis(N00H) \\sim Ueq, Uanis(C00T) \\sim Ueq,
Uanis(C015) \\sim Ueq, Uanis(C01E) \\sim Ueq, Uanis(C013) \\sim Ueq,
Uanis(C014) \\sim Ueq, Uanis(C01G) \\sim Ueq, Uanis(C011) \\sim Ueq,
Uanis(C016) \\sim Ueq, Uanis(C00Z) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
4.a Free rotating group:
 O1(H1A,H1B), O0AA(H0AA,H0AB)
4.b Ternary CH refined with riding coordinates:
 C00L(H00L), C00O(H00Q), C00T(H00T), C00U(H00U)
4.c Aromatic/amide H refined with riding coordinates:
 C00Q(H00Z), C00R(H00R), C00V(H00V), C00W(H00W), C00X(H00), C012(H012),
 C013(H013), C014(H014), C016(H016), C017(H017), C018(H018), C01C(H01D),
 C01F(H01I), C01G(H01H), C4(H4), C5(H5)
4.d Idealised Me refined as rotating group:
 N00H(H00J,H00K,H00M), C00I(H00D,H00E,H00F), N00J(H00N,H00O,H00P), N00K(H00G,
 H00H,H00I), N00M(H00A,H00B,H00C), C00P(H00S,H00X,H00Y), C010(H01A,H01B,H01C),
 C015(H01E,H01F,H01G)
;
_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
Pb01 Pb -0.02462(9) 0.49800(2) 1.12907(8) 0.0097(2) Uani 1 1 d . . . . .
Pb02 Pb 0.47951(9) 0.50429(2) 0.66075(8) 0.0100(2) Uani 1 1 d . . . . .
Br03 Br 0.1609(2) 0.49633(6) 1.4233(2) 0.0114(4) Uani 1 1 d . . . . .
Br04 Br 0.4712(2) 0.42300(7) 0.6319(2) 0.0113(5) Uani 1 1 d . . . . .
Br05 Br 0.6591(2) 0.50460(7) 0.3703(2) 0.0114(4) Uani 1 1 d . . . . .
Br06 Br 0.0166(3) 0.41482(7) 1.1329(2) 0.0117(5) Uani 1 1 d . . . . .
Br07 Br 0.5370(3) 0.58778(7) 0.6665(2) 0.0141(5) Uani 1 1 d . . . . .
Br08 Br -0.0359(3) 0.57989(7) 1.1627(2) 0.0122(5) Uani 1 1 d . . . . .
Br09 Br -0.1946(2) 0.49650(7) 0.8094(2) 0.0184(5) Uani 1 1 d . . . . .
Br0A Br 0.2966(2) 0.50225(8) 0.9800(2) 0.0183(5) Uani 1 1 d . . . . .
Br0B Br -0.1017(3) 0.72439(8) 0.8614(3) 0.0227(6) Uani 1 1 d . . . . .
Br0C Br 0.4826(3) 0.25071(7) 0.4740(3) 0.0242(6) Uani 1 1 d . . . . .
Br0D Br 0.4277(3) 0.27757(7) -0.0667(3) 0.0251(6) Uani 1 1 d . . . . .
Br0E Br 1.0347(3) 0.74966(8) 0.3314(3) 0.0301(6) Uani 1 1 d . . . . .
N00H N 1.080(2) 0.4019(5) -0.228(2) 0.014(4) Uani 1 1 d . U . . .
H00J H 0.993817 0.408894 -0.291633 0.017 Uiso 1 1 calc GR . . . .
H00K H 1.179915 0.411755 -0.258930 0.017 Uiso 1 1 calc GR . . . .
H00M H 1.057167 0.410332 -0.133447 0.017 Uiso 1 1 calc GR . . . .
C00I C 0.545(3) 0.4081(7) 0.025(2) 0.014(5) Uani 1 1 d . U . . .
H00D H 0.437784 0.396843 -0.009831 0.020 Uiso 1 1 calc GR . . . .
H00E H 0.641392 0.393981 -0.015533 0.020 Uiso 1 1 calc GR . . . .
H00F H 0.551109 0.433842 -0.010182 0.020 Uiso 1 1 calc GR . . . .
N00J N 0.925(2) 0.5674(5) 0.538(2) 0.008(4) Uani 1 1 d . U . . .
H00N H 0.955921 0.558091 0.447333 0.010 Uiso 1 1 calc GR . . . .
H00O H 0.827280 0.580794 0.526984 0.010 Uiso 1 1 calc GR . . . .
H00P H 0.907528 0.548312 0.603222 0.010 Uiso 1 1 calc GR . . . .
N00K N 0.417(2) 0.4326(5) 0.258(2) 0.010(4) Uani 1 1 d . U . . .
H00G H 0.434408 0.456034 0.223313 0.012 Uiso 1 1 calc GR . . . .
H00H H 0.420439 0.432621 0.360140 0.012 Uiso 1 1 calc GR . . . .
H00I H 0.313222 0.424276 0.225086 0.012 Uiso 1 1 calc GR . . . .
C00L C 0.555(3) 0.4073(6) 0.200(2) 0.011(4) Uani 1 1 d . U . . .
H00L H 0.668183 0.417126 0.233806 0.014 Uiso 1 1 calc R . . . .
N00M N 0.573(2) 0.6040(5) 1.022(2) 0.017(4) Uani 1 1 d . U . . .
H00A H 0.513955 0.595948 0.939566 0.020 Uiso 1 1 calc GR . . . .
H00B H 0.520343 0.596104 1.106564 0.020 Uiso 1 1 calc DGR . . . .
H00C H 0.681218 0.594785 1.020494 0.020 Uiso 1 1 calc GR . . . .
C00N C 0.532(2) 0.3689(6) 0.263(2) 0.010(4) Uani 1 1 d . U . . .
C00O C 1.068(2) 0.5925(6) 0.600(2) 0.008(4) Uani 1 1 d . U . . .
H00Q H 1.177810 0.581298 0.567478 0.010 Uiso 1 1 calc R . . . .
C00P C 1.068(3) 0.5910(7) 0.765(3) 0.018(5) Uani 1 1 d . U . . .
H00S H 0.963048 0.602352 0.802367 0.027 Uiso 1 1 calc GR . . . .
H00X H 1.167056 0.604568 0.805244 0.027 Uiso 1 1 calc GR . . . .
H00Y H 1.073859 0.565019 0.798050 0.027 Uiso 1 1 calc GR . . . .
C00Q C 1.200(3) 0.6459(7) 0.467(2) 0.015(5) Uani 1 1 d . U . . .
H00Z H 1.301146 0.631757 0.457537 0.019 Uiso 1 1 calc R . . . .
C00R C 0.266(3) 0.6548(7) 1.058(3) 0.016(5) Uani 1 1 d . U . . .
H00R H 0.270916 0.637770 1.139163 0.020 Uiso 1 1 calc DR . . . .
C00S C 1.061(2) 0.6302(6) 0.535(2) 0.011(4) Uani 1 1 d . U . . .
C00T C 1.093(3) 0.3602(6) -0.225(2) 0.014(5) Uani 1 1 d . U . . .
H00T H 1.182067 0.353445 -0.148514 0.017 Uiso 1 1 calc R . . . .
C00U C 0.580(3) 0.6462(6) 1.021(2) 0.013(5) Uani 1 1 d . U . . .
H00U H 0.667214 0.654195 0.947165 0.015 Uiso 1 1 calc R . . . .
C00V C 0.377(3) 0.3500(7) 0.258(3) 0.018(5) Uani 1 1 d . U . . .
H00V H 0.280733 0.361088 0.209314 0.022 Uiso 1 1 calc R . . . .
C00W C 0.659(3) 0.3152(6) 0.385(2) 0.011(4) Uani 1 1 d . U . . .
H00W H 0.754716 0.303063 0.429281 0.013 Uiso 1 1 calc R . . . .
C00X C 0.910(3) 0.6509(6) 0.544(2) 0.014(5) Uani 1 1 d . U . . .
H00 H 0.812708 0.640445 0.590151 0.017 Uiso 1 1 calc R . . . .
C00Y C 0.411(3) 0.6619(7) 0.973(2) 0.014(5) Uani 1 1 d . U . . .
C00Z C 0.503(3) 0.2980(7) 0.378(3) 0.022(5) Uani 1 1 d . U . . .
C010 C 0.635(3) 0.6604(7) 1.177(3) 0.022(5) Uani 1 1 d . U . . .
H01A H 0.551360 0.652719 1.251122 0.033 Uiso 1 1 calc GR . . . .
H01B H 0.642768 0.687564 1.174847 0.033 Uiso 1 1 calc GR . . . .
H01C H 0.747094 0.649932 1.203666 0.033 Uiso 1 1 calc GR . . . .
C011 C 0.628(3) 0.3050(7) -0.106(3) 0.017(5) Uani 1 1 d . U . . .
C012 C 0.630(3) 0.3285(7) -0.229(3) 0.020(5) Uani 1 1 d . U . . .
H012 H 0.529345 0.332300 -0.287994 0.024 Uiso 1 1 calc R . . . .
C013 C 0.781(3) 0.3466(6) -0.265(2) 0.012(4) Uani 1 1 d . U . . .
H013 H 0.783637 0.362131 -0.350707 0.015 Uiso 1 1 calc R . . . .
C014 C 0.923(3) 0.3189(6) -0.054(2) 0.013(5) Uani 1 1 d . U . . .
H014 H 1.022388 0.315784 0.006936 0.016 Uiso 1 1 calc R . . . .
C015 C 1.152(3) 0.3465(7) -0.374(2) 0.016(5) Uani 1 1 d . U . . .
H01E H 1.067966 0.352854 -0.452231 0.024 Uiso 1 1 calc GR . . . .
H01F H 1.166775 0.319432 -0.370180 0.024 Uiso 1 1 calc GR . . . .
H01G H 1.261935 0.358147 -0.397392 0.024 Uiso 1 1 calc GR . . . .
C016 C 0.673(3) 0.3509(7) 0.327(3) 0.019(5) Uani 1 1 d . U . . .
H016 H 0.780880 0.363077 0.330140 0.023 Uiso 1 1 calc R . . . .
C017 C 0.363(3) 0.3153(6) 0.322(2) 0.014(5) Uani 1 1 d . U . . .
H017 H 0.255047 0.303504 0.326064 0.017 Uiso 1 1 calc R . . . .
C018 C 0.114(3) 0.6730(7) 1.022(3) 0.021(5) Uani 1 1 d . U . . .
H018 H 0.015257 0.668779 1.080633 0.025 Uiso 1 1 calc R . . . .
C019 C 0.105(3) 0.6976(7) 0.900(2) 0.014(5) Uani 1 1 d . U . . .
C01A C 1.044(3) 0.7014(7) 0.421(3) 0.019(5) Uani 1 1 d . U . . .
C01C C 0.246(3) 0.7040(7) 0.815(3) 0.019(5) Uani 1 1 d . U . . .
H01D H 0.238729 0.720692 0.732134 0.023 Uiso 1 1 calc R . . . .
C01E C 0.927(3) 0.3424(7) -0.177(3) 0.018(5) Uani 1 1 d . U . . .
C01F C 1.195(3) 0.6817(7) 0.413(3) 0.015(5) Uani 1 1 d . U . . .
H01I H 1.293073 0.692583 0.370071 0.019 Uiso 1 1 calc R . . . .
C01G C 0.773(3) 0.2998(8) -0.017(3) 0.025(6) Uani 1 1 d . U . . .
H01H H 0.770507 0.283600 0.066911 0.030 Uiso 1 1 calc R . . . .
C4 C 0.399(3) 0.6864(7) 0.848(3) 0.021(5) Uani 1 1 d . U . . .
H4 H 0.495871 0.690674 0.787681 0.025 Uiso 1 1 calc R . . . .
C5 C 0.903(3) 0.6867(7) 0.486(3) 0.019(5) Uani 1 1 d . U . . .
H5 H 0.800356 0.700798 0.491167 0.023 Uiso 1 1 calc R . . . .
O1 O 0.3867(19) 0.5764(5) 1.2625(19) 0.021(4) Uani 1 1 d . . . . .
H1A H 0.386538 0.554509 1.220914 0.031 Uiso 1 1 d DG . . . .
H1B H 0.286450 0.586474 1.251302 0.031 Uiso 1 1 d DG . . . .
O0AA O 0.888(2) 0.4237(5) -0.475(2) 0.026(4) Uani 1 1 d . . . . .
H0AA H 0.782076 0.428978 -0.455387 0.039 Uiso 1 1 d G . . . .
H0AB H 0.929071 0.440525 -0.534272 0.039 Uiso 1 1 d G . . . .


_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 Br03 2.975(2) . ?
Pb01 Br06 3.010(3) . ?
Pb01 Br08 2.963(3) . ?
Pb01 Br09 3.122(2) . ?
Pb01 Br0A 2.867(2) . ?
Pb02 Br04 2.937(3) . ?
Pb02 Br05 2.9626(19) . ?
Pb02 Br07 3.038(3) . ?
Pb02 Br09 2.871(2) 1_655 ?
Pb02 Br0A 3.203(2) . ?
Br0B C019 1.91(2) . ?
Br0C C00Z 1.91(3) . ?
Br0D C011 1.89(2) . ?
Br0E C01A 1.91(2) . ?
N00H C00T 1.51(3) . ?
C00I C00L 1.56(3) . ?
N00J C00O 1.53(3) . ?
N00K C00L 1.51(3) . ?
C00L C00N 1.50(3) . ?
N00M C00U 1.52(3) . ?
C00N C00V 1.39(3) . ?
C00N C016 1.39(3) . ?
C00O C00P 1.47(3) . ?
C00O C00S 1.48(3) . ?
C00Q C00S 1.37(3) . ?
C00Q C01F 1.37(3) . ?
C00R C00Y 1.40(3) . ?
C00R C018 1.39(3) . ?
C00S C00X 1.40(3) . ?
C00T C015 1.50(3) . ?
C00T C01E 1.51(3) . ?
C00U C00Y 1.50(3) . ?
C00U C010 1.53(3) . ?
C00V C017 1.38(3) . ?
C00W C00Z 1.37(3) . ?
C00W C016 1.39(3) . ?
C00X C5 1.39(3) . ?
C00Y C4 1.42(3) . ?
C00Z C017 1.35(3) . ?
C011 C012 1.38(3) . ?
C011 C01G 1.38(3) . ?
C012 C013 1.39(3) . ?
C013 C01E 1.38(3) . ?
C014 C01E 1.39(3) . ?
C014 C01G 1.41(3) . ?
C018 C019 1.40(3) . ?
C019 C01C 1.37(3) . ?
C01A C01F 1.38(3) . ?
C01A C5 1.37(3) . ?
C01C C4 1.38(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
Br03 Pb01 Br06 85.37(6) . . ?
Br03 Pb01 Br09 175.46(6) . . ?
Br06 Pb01 Br09 92.13(7) . . ?
Br08 Pb01 Br03 86.92(6) . . ?
Br08 Pb01 Br06 172.25(6) . . ?
Br08 Pb01 Br09 95.52(7) . . ?
Br0A Pb01 Br03 89.31(6) . . ?
Br0A Pb01 Br06 87.91(7) . . ?
Br0A Pb01 Br08 91.24(7) . . ?
Br0A Pb01 Br09 86.81(6) . . ?
Br04 Pb02 Br05 86.42(6) . . ?
Br04 Pb02 Br07 171.64(6) . . ?
Br04 Pb02 Br0A 92.59(7) . . ?
Br05 Pb02 Br07 86.47(7) . . ?
Br05 Pb02 Br0A 177.92(7) . . ?
Br07 Pb02 Br0A 94.37(7) . . ?
Br09 Pb02 Br04 87.79(7) 1_655 . ?
Br09 Pb02 Br05 88.34(6) 1_655 . ?
Br09 Pb02 Br07 87.60(7) 1_655 . ?
Br09 Pb02 Br0A 89.79(6) 1_655 . ?
Pb02 Br09 Pb01 141.41(8) 1_455 . ?
Pb01 Br0A Pb02 145.07(8) . . ?
N00K C00L C00I 108.0(16) . . ?
C00N C00L C00I 112.8(18) . . ?
C00N C00L N00K 109.8(16) . . ?
C00V C00N C00L 122.7(19) . . ?
C00V C00N C016 118(2) . . ?
C016 C00N C00L 118.9(18) . . ?
C00P C00O N00J 109.0(17) . . ?
C00P C00O C00S 115.3(19) . . ?
C00S C00O N00J 112.3(17) . . ?
C00S C00Q C01F 121(2) . . ?
C018 C00R C00Y 119(2) . . ?
C00Q C00S C00O 121.7(19) . . ?
C00Q C00S C00X 119(2) . . ?
C00X C00S C00O 119.5(18) . . ?
N00H C00T C01E 111.7(17) . . ?
C015 C00T N00H 109.8(18) . . ?
C015 C00T C01E 113.0(19) . . ?
N00M C00U C010 109.8(18) . . ?
C00Y C00U N00M 110.3(18) . . ?
C00Y C00U C010 111.8(19) . . ?
C017 C00V C00N 120(2) . . ?
C00Z C00W C016 119(2) . . ?
C5 C00X C00S 120(2) . . ?
C00R C00Y C00U 120(2) . . ?
C00R C00Y C4 119(2) . . ?
C4 C00Y C00U 120.4(19) . . ?
C00W C00Z Br0C 117.8(18) . . ?
C017 C00Z Br0C 120.2(18) . . ?
C017 C00Z C00W 122(2) . . ?
C012 C011 Br0D 118.9(17) . . ?
C01G C011 Br0D 119.9(18) . . ?
C01G C011 C012 121(2) . . ?
C011 C012 C013 119(2) . . ?
C01E C013 C012 121(2) . . ?
C01E C014 C01G 121(2) . . ?
C00W C016 C00N 121(2) . . ?
C00Z C017 C00V 120(2) . . ?
C00R C018 C019 120(2) . . ?
C018 C019 Br0B 119.2(16) . . ?
C01C C019 Br0B 120.2(18) . . ?
C01C C019 C018 120(2) . . ?
C01F C01A Br0E 118.3(17) . . ?
C5 C01A Br0E 120.0(18) . . ?
C5 C01A C01F 122(2) . . ?
C019 C01C C4 120(2) . . ?
C013 C01E C00T 120(2) . . ?
C013 C01E C014 119(2) . . ?
C014 C01E C00T 121(2) . . ?
C00Q C01F C01A 119(2) . . ?
C011 C01G C014 119(2) . . ?
C01C C4 C00Y 120(2) . . ?
C01A C5 C00X 119(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 3.047
_oxdiff_exptl_absorpt_empirical_full_min 0.507

# start Validation Reply Form
_vrf_PLAT342_pbbr-4-brmba        
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.03062 Ang.  
RESPONSE: Caused by the absorption of heavier atoms present in the 
structure
;
_vrf_PLAT971_pbbr-4-brmba        
;
PROBLEM: Check Calcd Resid. Dens.  1.22Ang From Pb01            3.10 eA-3  
RESPONSE: This is mainly caused by the Fourier truncation error for
the heavy metal element.
;
_vrf_PLAT972_pbbr-4-brmba        
;
PROBLEM: Check Calcd Resid. Dens.  2.33Ang From Br0A           -2.67 eA-3  
RESPONSE: This is mainly caused by the Fourier truncation error for
the heavy metal element.
;
# 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_zixuan49a_173k_auto
_database_code_depnum_ccdc_archive 'CCDC 2348608'
loop_
_audit_author_name
_audit_author_address
'ZIXUAN ZHANG'
;Hong Kong University of Science and Technology
Hong Kong
;
_audit_update_record             
;
2024-04-16 deposited with the CCDC.	2024-10-30 downloaded from the CCDC.
;
_audit_creation_date             2023-12-07
_audit_creation_method           
;
Olex2 1.5-alpha
(compiled 2023.11.24 svn.r209d9fb2 for OlexSys, GUI svn.r6869)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'I4 Pb, 2(C8 H11 Br N)'
_chemical_formula_sum            'C16 H22 Br2 I4 N2 Pb'
_chemical_formula_weight         1116.96
_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 0.0181 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'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 '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'
Pb Pb -4.0753 8.5060 '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           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   9.1768(2)
_cell_length_b                   8.2407(2)
_cell_length_c                   17.8463(5)
_cell_angle_alpha                90
_cell_angle_beta                 98.883(2)
_cell_angle_gamma                90
_cell_volume                     1333.40(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4917
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      74.0610
_cell_measurement_theta_min      4.8740
_shelx_estimated_absorpt_T_max   0.422
_shelx_estimated_absorpt_T_min   0.303
_exptl_absorpt_coefficient_mu    52.197
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66664
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.782
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0437
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            7755
_diffrn_reflns_point_group_measured_fraction_full 0.853
_diffrn_reflns_point_group_measured_fraction_max 0.817
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.263
_diffrn_reflns_theta_min         4.878
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3577
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     13.00 116.00   1.00    4.00    --   39.70  37.00   0.00  103
  2  ω     12.00 106.00   1.00    4.00    --   39.70  57.00-120.00   94
  3  ω    -21.00  71.00   1.00    4.00    --   39.70 -77.00  90.00   92
  4  ω     80.00 127.00   1.00   11.00    --  107.44  45.00 120.00   47
  5  ω     77.00 158.00   1.00   11.00    --  107.44  61.00   0.00   81
  6  ω     32.00 103.00   1.00   11.00    --  107.44 -94.00 -30.00   71
  7  ω    104.00 178.00   1.00   11.00    --  107.44 111.00  30.00   74
  8  ω     80.00 116.00   1.00   11.00    --  107.44  45.00  90.00   36
  9  ω    127.00 170.00   1.00   11.00    --  107.44  45.00  90.00   43
 10  ω     39.00 108.00   1.00   11.00    --  107.44-111.00-120.00   69
 11  ω    139.00 178.00   1.00   11.00    --  107.44  45.00 120.00   39
 12  ω     29.00 141.00   1.00   11.00    --  107.44 -77.00  30.00  112
 13  ω     33.00  99.00   1.00   11.00    --  107.44 -30.00  90.00   66
 14  ω    113.00 138.00   1.00   11.00    --  107.44 -30.00  90.00   25
 15  ω    108.00 133.00   1.00   11.00    --  107.44 111.00-180.00   25
;
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1512581000
_diffrn_orient_matrix_UB_12      0.0023984000
_diffrn_orient_matrix_UB_13      0.0273098000
_diffrn_orient_matrix_UB_21      0.0753700000
_diffrn_orient_matrix_UB_22      0.0480140000
_diffrn_orient_matrix_UB_23      0.0801174000
_diffrn_orient_matrix_UB_31      -0.0181100000
_diffrn_orient_matrix_UB_32      0.1806027000
_diffrn_orient_matrix_UB_33      -0.0216886000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           0.80
_diffrn_source_power             0.040
_diffrn_source_target            Cu
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_source_voltage           50
_reflns_Friedel_coverage         0.565
_reflns_Friedel_fraction_full    0.685
_reflns_Friedel_fraction_max     0.636
_reflns_number_gt                4199
_reflns_number_total             4452
_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 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5-alpha (Bourhis et al., 2015)'
_refine_diff_density_max         1.043
_refine_diff_density_min         -0.830
_refine_diff_density_rms         0.148
_refine_ls_abs_structure_details 
;
 Flack x determined using 1421 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.004(9)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         4452
_refine_ls_number_restraints     55
_refine_ls_R_factor_all          0.0280
_refine_ls_R_factor_gt           0.0251
_refine_ls_restrained_S_all      1.004
_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)+(0.0207P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0548
_refine_ls_wR_factor_ref         0.0559
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12)
\\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C17) \\sim Ueq,
Uanis(C18) \\sim Ueq, Uanis(N2) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.01
3.a Ternary CH refined with riding coordinates:
 C17(H17), C7(H7)
3.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C14(H14), C15(H15), C16(H16), C2(H2), C4(H4), C5(H5), C6(H6)
3.c Idealised Me refined as rotating group:
 N2(H2A,H2B,H2C), C18(H18A,H18B,H18C), N1(H1A,H1B,H1C), C8(H8A,H8B,H8C)
;
_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 0.74943(4) 0.31981(5) 0.49896(2) 0.01509(8) Uani 1 1 d . . . . .
I1 I 0.66537(7) 0.37552(8) 0.32092(4) 0.02171(15) Uani 1 1 d . . . . .
I2 I 0.57236(7) -0.01775(7) 0.48034(4) 0.01932(13) Uani 1 1 d . . . . .
I3 I 0.82542(6) 0.32912(8) 0.67882(3) 0.01873(13) Uani 1 1 d . . . . .
I4 I 0.95346(7) 0.63456(7) 0.51084(4) 0.02264(14) Uani 1 1 d . . . . .
Br2 Br 0.8635(2) 0.43238(18) 0.08246(8) 0.0541(4) Uani 1 1 d . . . . .
N2 N 0.7861(9) 0.8093(11) 0.3346(5) 0.0232(17) Uani 1 1 d . U . . .
H2A H 0.757146 0.703751 0.329673 0.028 Uiso 1 1 calc R U . . .
H2B H 0.754941 0.853118 0.376137 0.028 Uiso 1 1 calc R U . . .
H2C H 0.886244 0.814850 0.339966 0.028 Uiso 1 1 calc R U . . .
C11 C 0.7978(12) 0.8533(12) 0.1978(6) 0.024(2) Uani 1 1 d . U . . .
C12 C 0.7951(12) 0.6920(13) 0.1743(6) 0.024(2) Uani 1 1 d . U . . .
H12 H 0.743154 0.611908 0.197880 0.028 Uiso 1 1 calc R U . . .
C13 C 0.8695(12) 0.6527(15) 0.1163(6) 0.029(2) Uani 1 1 d . U . . .
C14 C 0.9487(15) 0.7627(17) 0.0799(8) 0.041(3) Uani 1 1 d . U . . .
H14 H 1.002673 0.731020 0.040948 0.049 Uiso 1 1 calc R U . . .
C15 C 0.9439(15) 0.9236(18) 0.1044(8) 0.044(3) Uani 1 1 d . U . . .
H15 H 0.991574 1.005169 0.079341 0.053 Uiso 1 1 calc R U . . .
C16 C 0.8730(13) 0.9669(15) 0.1629(7) 0.032(2) Uani 1 1 d . U . . .
H16 H 0.875790 1.076482 0.179633 0.039 Uiso 1 1 calc R U . . .
C17 C 0.7186(12) 0.9044(14) 0.2634(6) 0.026(2) Uani 1 1 d . U . . .
H17 H 0.735746 1.022918 0.273186 0.032 Uiso 1 1 calc R U . . .
C18 C 0.5546(14) 0.8729(19) 0.2502(9) 0.046(3) Uani 1 1 d . U . . .
H18A H 0.536355 0.757935 0.238291 0.069 Uiso 1 1 calc R U . . .
H18B H 0.507673 0.939514 0.207749 0.069 Uiso 1 1 calc R U . . .
H18C H 0.513390 0.900879 0.296036 0.069 Uiso 1 1 calc R U . . .
Br1 Br 0.3703(2) 0.6502(2) 0.04478(9) 0.0576(4) Uani 1 1 d . . . . .
N1 N 0.3067(9) 0.2445(10) 0.3465(5) 0.0188(17) Uani 1 1 d . . . . .
H1A H 0.264850 0.145656 0.335135 0.023 Uiso 1 1 calc R U . . .
H1B H 0.296199 0.272146 0.394795 0.023 Uiso 1 1 calc R U . . .
H1C H 0.404232 0.240193 0.342517 0.023 Uiso 1 1 calc R U . . .
C1 C 0.2684(11) 0.3423(13) 0.2126(6) 0.021(2) Uani 1 1 d . . . . .
C2 C 0.2986(12) 0.4802(15) 0.1726(6) 0.028(2) Uani 1 1 d . . . . .
H2 H 0.297245 0.584870 0.194864 0.033 Uiso 1 1 calc R U . . .
C3 C 0.3307(12) 0.4616(16) 0.1000(6) 0.029(2) Uani 1 1 d . . . . .
C4 C 0.3359(13) 0.3114(18) 0.0668(7) 0.035(3) Uani 1 1 d . . . . .
H4 H 0.362232 0.299622 0.017632 0.042 Uiso 1 1 calc R U . . .
C5 C 0.3007(14) 0.1763(16) 0.1085(7) 0.034(3) Uani 1 1 d . . . . .
H5 H 0.298985 0.071576 0.086164 0.041 Uiso 1 1 calc R U . . .
C6 C 0.2689(13) 0.1921(13) 0.1805(6) 0.027(2) Uani 1 1 d . . . . .
H6 H 0.247175 0.098878 0.208101 0.032 Uiso 1 1 calc R U . . .
C7 C 0.2317(11) 0.3694(11) 0.2923(6) 0.019(2) Uani 1 1 d . . . . .
H7 H 0.270119 0.478632 0.310005 0.023 Uiso 1 1 calc R U . . .
C8 C 0.0662(12) 0.3660(13) 0.2954(7) 0.029(3) Uani 1 1 d . . . . .
H8A H 0.028666 0.255549 0.285291 0.043 Uiso 1 1 calc R U . . .
H8B H 0.015185 0.440094 0.257150 0.043 Uiso 1 1 calc R U . . .
H8C H 0.048712 0.400100 0.345894 0.043 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 I1 3.1849(8) . ?
Pb1 I2 3.3144(7) 2_656 ?
Pb1 I2 3.2128(7) . ?
Pb1 I3 3.1787(7) . ?
Pb1 I4 3.1531(7) 2_746 ?
Pb1 I4 3.1868(7) . ?
Br2 C13 1.912(12) . ?
N2 H2A 0.9100 . ?
N2 H2B 0.9100 . ?
N2 H2C 0.9100 . ?
N2 C17 1.538(14) . ?
C11 C12 1.393(15) . ?
C11 C16 1.369(15) . ?
C11 C17 1.530(15) . ?
C12 H12 0.9500 . ?
C12 C13 1.364(16) . ?
C13 C14 1.385(18) . ?
C14 H14 0.9500 . ?
C14 C15 1.40(2) . ?
C15 H15 0.9500 . ?
C15 C16 1.361(19) . ?
C16 H16 0.9500 . ?
C17 H17 1.0000 . ?
C17 C18 1.509(16) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
Br1 C3 1.905(11) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 H1C 0.9100 . ?
N1 C7 1.505(13) . ?
C1 C2 1.391(16) . ?
C1 C6 1.364(15) . ?
C1 C7 1.528(14) . ?
C2 H2 0.9500 . ?
C2 C3 1.382(15) . ?
C3 C4 1.376(19) . ?
C4 H4 0.9500 . ?
C4 C5 1.404(19) . ?
C5 H5 0.9500 . ?
C5 C6 1.368(16) . ?
C6 H6 0.9500 . ?
C7 H7 1.0000 . ?
C7 C8 1.529(13) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 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
I1 Pb1 I2 88.906(19) . . ?
I1 Pb1 I2 88.296(19) . 2_656 ?
I1 Pb1 I4 89.91(2) . . ?
I2 Pb1 I2 85.188(11) . 2_656 ?
I3 Pb1 I1 170.22(2) . . ?
I3 Pb1 I2 98.85(2) . . ?
I3 Pb1 I2 86.444(18) . 2_656 ?
I3 Pb1 I4 83.00(2) . . ?
I4 Pb1 I1 95.32(2) 2_746 . ?
I4 Pb1 I2 173.81(2) . . ?
I4 Pb1 I2 100.852(19) . 2_656 ?
I4 Pb1 I2 174.06(2) 2_746 2_656 ?
I4 Pb1 I2 90.169(19) 2_746 . ?
I4 Pb1 I3 90.627(19) 2_746 . ?
I4 Pb1 I4 83.889(10) 2_746 . ?
Pb1 I2 Pb1 141.56(2) . 2_646 ?
Pb1 I4 Pb1 153.45(2) 2_756 . ?
H2A N2 H2B 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
C17 N2 H2A 109.5 . . ?
C17 N2 H2B 109.5 . . ?
C17 N2 H2C 109.5 . . ?
C12 C11 C17 120.3(10) . . ?
C16 C11 C12 120.1(11) . . ?
C16 C11 C17 119.5(10) . . ?
C11 C12 H12 121.1 . . ?
C13 C12 C11 117.9(10) . . ?
C13 C12 H12 121.1 . . ?
C12 C13 Br2 118.1(8) . . ?
C12 C13 C14 124.1(12) . . ?
C14 C13 Br2 117.7(9) . . ?
C13 C14 H14 122.3 . . ?
C13 C14 C15 115.4(13) . . ?
C15 C14 H14 122.3 . . ?
C14 C15 H15 119.0 . . ?
C16 C15 C14 122.0(13) . . ?
C16 C15 H15 119.0 . . ?
C11 C16 H16 119.9 . . ?
C15 C16 C11 120.3(12) . . ?
C15 C16 H16 119.9 . . ?
N2 C17 H17 108.7 . . ?
C11 C17 N2 108.2(9) . . ?
C11 C17 H17 108.7 . . ?
C18 C17 N2 107.8(10) . . ?
C18 C17 C11 114.4(10) . . ?
C18 C17 H17 108.7 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C7 N1 H1A 109.5 . . ?
C7 N1 H1B 109.5 . . ?
C7 N1 H1C 109.5 . . ?
C2 C1 C7 116.6(9) . . ?
C6 C1 C2 120.9(10) . . ?
C6 C1 C7 122.6(10) . . ?
C1 C2 H2 120.7 . . ?
C3 C2 C1 118.5(11) . . ?
C3 C2 H2 120.7 . . ?
C2 C3 Br1 118.7(10) . . ?
C4 C3 Br1 119.3(9) . . ?
C4 C3 C2 122.1(11) . . ?
C3 C4 H4 121.4 . . ?
C3 C4 C5 117.3(10) . . ?
C5 C4 H4 121.4 . . ?
C4 C5 H5 119.2 . . ?
C6 C5 C4 121.5(12) . . ?
C6 C5 H5 119.2 . . ?
C1 C6 C5 119.7(11) . . ?
C1 C6 H6 120.2 . . ?
C5 C6 H6 120.2 . . ?
N1 C7 C1 110.8(8) . . ?
N1 C7 H7 108.0 . . ?
N1 C7 C8 108.8(8) . . ?
C1 C7 H7 108.0 . . ?
C1 C7 C8 113.2(9) . . ?
C8 C7 H7 108.0 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Br2 C13 C14 C15 177.1(10) . . . . ?
C11 C12 C13 Br2 -178.9(8) . . . . ?
C11 C12 C13 C14 0.7(18) . . . . ?
C12 C11 C16 C15 0.9(18) . . . . ?
C12 C11 C17 N2 60.0(13) . . . . ?
C12 C11 C17 C18 -60.2(15) . . . . ?
C12 C13 C14 C15 -2(2) . . . . ?
C13 C14 C15 C16 4(2) . . . . ?
C14 C15 C16 C11 -3(2) . . . . ?
C16 C11 C12 C13 0.2(17) . . . . ?
C16 C11 C17 N2 -119.1(11) . . . . ?
C16 C11 C17 C18 120.6(13) . . . . ?
C17 C11 C12 C13 -179.0(10) . . . . ?
C17 C11 C16 C15 -179.9(11) . . . . ?
Br1 C3 C4 C5 -177.8(9) . . . . ?
C1 C2 C3 Br1 179.4(8) . . . . ?
C1 C2 C3 C4 -1.1(17) . . . . ?
C2 C1 C6 C5 0.6(17) . . . . ?
C2 C1 C7 N1 -138.0(9) . . . . ?
C2 C1 C7 C8 99.5(11) . . . . ?
C2 C3 C4 C5 2.8(17) . . . . ?
C3 C4 C5 C6 -2.8(18) . . . . ?
C4 C5 C6 C1 1.2(19) . . . . ?
C6 C1 C2 C3 -0.7(16) . . . . ?
C6 C1 C7 N1 43.4(13) . . . . ?
C6 C1 C7 C8 -79.1(13) . . . . ?
C7 C1 C2 C3 -179.3(10) . . . . ?
C7 C1 C6 C5 179.1(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 1.699
_oxdiff_exptl_absorpt_empirical_full_min 0.703
