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

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

data_impbbr3_024gpa
_database_code_depnum_ccdc_archive 'CCDC 2473957'
loop_
_audit_author_name
_audit_author_address
'Kinga Roszak'
;Adam Mickiewicz University Poznan
Poland
;
_audit_update_record             
;
2025-07-18 deposited with the CCDC.	2026-03-26 downloaded from the CCDC.
;
_audit_creation_date             2024-07-31
# start Validation Reply Form
_vrf_PLAT027_impbbr3_024gpa      
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      15.00 Degree
RESPONSE: A full set of data was collected, however 
the very high angle data was poor and was omitted.
Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the 
X-ray radiation to the measured sample.
;
_vrf_PLAT029_impbbr3_024gpa      
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.397 Why?  
RESPONSE: The data come from high-pressure studies and are 
limited by the DAC opening angle.
;
_vrf_PLAT090_impbbr3_024gpa      
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       3.47 Note  
RESPONSE: The data/parameter ratio is affected by the access limits of the DAC.
;
_vrf_PLAT342_impbbr3_024gpa      
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............       0.15 Ang.  
RESPONSE: Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the X-ray 
radiation to the measured sample; poor quality of measurement
;
_vrf_PLAT234_impbbr3_024gpa      
;
PROBLEM: Large Hirshfeld Difference Pb2      --Br1_d    .       0.26 Ang.  
RESPONSE: poor quality of measurement
;
_vrf_PLAT987_impbbr3_024gpa      
;
PROBLEM: The Flack x is >> 0 -  Do a BASF/TWIN Refinement     Please Check 
RESPONSE: The structure was refined as an inversion twin.
;
# end Validation Reply Form
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br3 Pb, C3 H5 N2'
_chemical_formula_sum            'C3 H5 Br3 N2 Pb'
_chemical_formula_weight         516.01
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z+1/2'

_cell_length_a                   14.1683(9)
_cell_length_b                   8.852(11)
_cell_length_c                   14.8432(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1862(2)
_cell_formula_units_Z            8
_cell_measurement_pressure       240000
_cell_measurement_reflns_used    2044
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.6650
_cell_measurement_theta_min      4.8670
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    30.932
_exptl_absorpt_correction_T_max  0.00746
_exptl_absorpt_correction_T_min  0.00104
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.89a (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    3.682
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0638
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_Laue_measured_fraction_full 0.397
_diffrn_reflns_Laue_measured_fraction_max 0.271
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       2
_diffrn_reflns_limit_k_min       -2
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7698
_diffrn_reflns_point_group_measured_fraction_full 0.406
_diffrn_reflns_point_group_measured_fraction_max 0.274
_diffrn_reflns_theta_full        15.000
_diffrn_reflns_theta_max         26.428
_diffrn_reflns_theta_min         4.596
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.2413
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.397
_diffrn_measured_fraction_theta_max 0.271
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  19.75   0.75   35.00   0.00 -30.00   0.00    --    73
  2  φ    140.00 200.00   0.75   35.00   0.00 -30.00   0.00    --    80
  3  φ    160.00 217.00   0.75   35.00   0.00  30.00   0.00    --    76
  4  φ    -20.00  34.75   0.75   35.00   0.00  30.00   0.00    --    73
  5  ω    -24.00  24.00   0.75   35.00    --   30.00  39.46 -12.90   64
  6  ω    -24.00  24.00   0.75   35.00    --   30.00  39.46 167.10   64
  7  ω    -50.00  10.00   0.75   35.00    --  -30.00  39.46 167.10   80
  8  ω    -50.00  10.00   0.75   35.00    --  -30.00  39.46 -12.90   80
  9  ω    -64.00  -8.50   0.75   35.00    --  -30.00  81.40 -28.90   74
 10  ω    -64.00  -8.50   0.75   35.00    --  -30.00  81.40 151.10   74
 11  ω    -19.00   8.00   0.75   35.00    --   30.00  81.40 151.10   36
 12  ω    -19.00   8.00   0.75   35.00    --   30.00  81.40 -28.90   36
 13  ω    -43.00 -21.25   0.75   35.00    --   30.00 134.60 -56.90   29
 14  ω    -43.00 -21.25   0.75   35.00    --   30.00 134.60 123.10   29
 15  ω    -90.00 -36.00   0.75   35.00    --  -30.00 134.60 123.10   72
 16  ω    -90.00 -36.00   0.75   35.00    --  -30.00 134.60 -56.90   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.946
_reflns_Friedel_fraction_full    0.416
_reflns_Friedel_fraction_max     0.278
_reflns_number_gt                669
_reflns_number_total             1022
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.003
_refine_diff_density_min         -0.599
_refine_diff_density_rms         0.205
_refine_ls_abs_structure_details 
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack   0.5
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         1022
_refine_ls_number_restraints     178
_refine_ls_R_factor_all          0.1016
_refine_ls_R_factor_gt           0.0655
_refine_ls_restrained_S_all      1.039
_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)+(0.1136P)²+3.3347P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1641
_refine_ls_wR_factor_ref         0.1933
_refine_special_details          
;
 Refined as a 2-component perfect inversion twin.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 N3-C4
 1.33 with sigma of 0.02
 N2-N1
 2.07 with sigma of 0.02
 C3-C1 \\sim C6-C5
 with sigma of 0.02
 N3-C4 \\sim N3-C6 \\sim N4-C5 \\sim N4-C4 \\sim N2-C2 \\sim N2-C3 \\sim N1-C1
\\sim N1-C2
 with sigma of 0.02
3. Restrained planarity
 C2, N1, C1, C3, N2
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(Br6) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(N3) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(N1) \\sim
Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of
0.004 and sigma for terminal atoms of 0.008
Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of
0.004 and sigma for terminal atoms of 0.008
Uanis(C1) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(Br1) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(Pb1) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(Br3) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.008
5. Rigid body (RIGU) restrains
 Pb1, Br2, Br1, Br5, Br4, Pb2, Br3, Br6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a :
 C6(C5,N4,C4,N3)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C1(H1), N1(H1A), C2(H2), N2(H2A), C6(H6), C5(H5), N4(H4), C4(H4A),
 N3(H3A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.1716(5) 0.015(3) 0.36577(16) 0.068(3) Uani 1 1 d . U . . .
Pb2 Pb 0.1720(5) 0.018(3) 0.62847(19) 0.122(11) Uani 1 1 d . . . . .
Br1 Br 0.2368(17) 0.270(7) 0.2560(11) 0.088(7) Uani 1 1 d . U . . .
Br2 Br 0.0698(4) 0.211(3) 0.4968(18) 0.116(15) Uani 1 1 d . . . . .
Br3 Br -0.002(2) 0.002(8) 0.7441(19) 0.079(2) Uani 1 1 d . U . . .
Br4 Br 0.3313(4) 0.052(2) 0.497(2) 0.115(16) Uani 1 1 d . . . . .
Br5 Br 0.1168(5) -0.230(3) 0.5004(17) 0.111(13) Uani 1 1 d . . . . .
Br6 Br 0.2358(16) 0.299(7) 0.7395(11) 0.087(6) Uani 1 1 d . U . . .
C3 C 0.364(6) 0.68(2) 0.438(5) 0.09(3) Uani 1 1 d D U . . .
H3 H 0.383729 0.758323 0.399236 0.103 Uiso 1 1 calc R U . . .
C1 C 0.378(6) 0.67(2) 0.523(4) 0.09(3) Uani 1 1 d D U . . .
H1 H 0.413775 0.733562 0.556948 0.112 Uiso 1 1 calc R U . . .
N1 N 0.336(7) 0.55(2) 0.558(7) 0.10(4) Uani 1 1 d D U . . .
H1A H 0.336413 0.518790 0.613341 0.122 Uiso 1 1 calc R U . . .
C2 C 0.292(6) 0.473(16) 0.491(10) 0.14(4) Uani 1 1 d D U . . .
H2 H 0.255097 0.385920 0.493114 0.174 Uiso 1 1 calc R U . . .
N2 N 0.315(6) 0.56(2) 0.420(7) 0.09(3) Uani 1 1 d D U . . .
H2A H 0.299445 0.532797 0.365749 0.109 Uiso 1 1 calc R U . . .
C6 C 0.497(6) 0.09(2) 0.303(5) 0.06(2) Uani 1 1 d DG U . . .
H6 H 0.488792 0.144830 0.354179 0.076 Uiso 1 1 calc R U . . .
C5 C 0.546(5) -0.04(2) 0.297(4) 0.09(3) Uani 1 1 d DG U . . .
H5 H 0.579673 -0.081606 0.343025 0.106 Uiso 1 1 calc R U . . .
N4 N 0.540(5) -0.09(2) 0.211(5) 0.09(3) Uani 1 1 d DG U . . .
H4 H 0.566697 -0.166535 0.190202 0.107 Uiso 1 1 calc R U . . .
C4 C 0.487(6) 0.00(2) 0.164(4) 0.11(4) Uani 1 1 d DG U . . .
H4A H 0.471505 -0.004240 0.103059 0.131 Uiso 1 1 calc R U . . .
N3 N 0.461(5) 0.11(2) 0.221(7) 0.12(4) Uani 1 1 d DG U . . .
H3A H 0.425239 0.185646 0.207094 0.145 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 2.93(5) . ?
Pb1 Br2 2.98(3) . ?
Pb1 Br3 3.01(3) 2_554 ?
Pb1 Br4 3.01(2) . ?
Pb1 Br5 3.05(3) . ?
Pb1 Br6 2.98(5) 4_544 ?
Pb2 Br1 3.17(5) 4_545 ?
Pb2 Br2 2.97(3) . ?
Pb2 Br3 3.01(3) . ?
Pb2 Br4 3.00(2) . ?
Pb2 Br5 3.01(3) . ?
Pb2 Br6 3.12(5) . ?
C3 H3 0.9300 . ?
C3 C1 1.29(4) . ?
C3 N2 1.33(4) . ?
C1 H1 0.9100 . ?
C1 N1 1.33(4) . ?
N1 H1A 0.8600 . ?
N1 C2 1.34(4) . ?
C2 H2 0.9300 . ?
C2 N2 1.33(4) . ?
N2 H2A 0.8600 . ?
C6 H6 0.9100 . ?
C6 C5 1.28(3) . ?
C6 N3 1.34(3) . ?
C5 H5 0.9100 . ?
C5 N4 1.36(3) . ?
N4 H4 0.8400 . ?
N4 C4 1.30(3) . ?
C4 H4A 0.9300 . ?
C4 N3 1.32(3) . ?
N3 H3A 0.8600 . ?

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 93.9(10) . . ?
Br1 Pb1 Br3 87.5(12) . 2_554 ?
Br1 Pb1 Br4 92.3(7) . . ?
Br1 Pb1 Br5 172.6(8) . . ?
Br1 Pb1 Br6 90.4(16) . 4_544 ?
Br2 Pb1 Br3 91.9(10) . 2_554 ?
Br2 Pb1 Br4 82.9(6) . . ?
Br2 Pb1 Br5 82.1(7) . . ?
Br2 Pb1 Br6 175.5(13) . 4_544 ?
Br3 Pb1 Br5 98.9(12) 2_554 . ?
Br4 Pb1 Br3 174.8(13) . 2_554 ?
Br4 Pb1 Br5 81.0(6) . . ?
Br6 Pb1 Br3 86.7(12) 4_544 2_554 ?
Br6 Pb1 Br4 98.5(6) 4_544 . ?
Br6 Pb1 Br5 93.8(11) 4_544 . ?
Br2 Pb2 Br1 171.2(12) . 4_545 ?
Br2 Pb2 Br3 90.2(10) . . ?
Br2 Pb2 Br4 83.2(6) . . ?
Br2 Pb2 Br5 83.0(7) . . ?
Br2 Pb2 Br6 91.7(10) . . ?
Br3 Pb2 Br1 87.7(12) . 4_545 ?
Br3 Pb2 Br5 96.5(12) . . ?
Br3 Pb2 Br6 88.5(13) . . ?
Br4 Pb2 Br1 98.7(6) . 4_545 ?
Br4 Pb2 Br3 173.3(10) . . ?
Br4 Pb2 Br5 81.9(6) . . ?
Br4 Pb2 Br6 92.6(7) . . ?
Br5 Pb2 Br1 88.8(11) . 4_545 ?
Br5 Pb2 Br6 172.7(9) . . ?
Br6 Pb2 Br1 96.8(15) . 4_545 ?
Pb1 Br1 Pb2 172.7(15) . 4_554 ?
Pb2 Br2 Pb1 81.8(5) . . ?
Pb2 Br3 Pb1 178.0(11) . 2 ?
Pb2 Br4 Pb1 81.04(16) . . ?
Pb2 Br5 Pb1 80.1(6) . . ?
Pb1 Br6 Pb2 166.4(16) 4 . ?
C1 C3 H3 127.0 . . ?
C1 C3 N2 101(10) . . ?
N2 C3 H3 129.5 . . ?
C3 C1 H1 126.0 . . ?
C3 C1 N1 113(10) . . ?
N1 C1 H1 122.0 . . ?
C1 N1 H1A 129.0 . . ?
C1 N1 C2 108(10) . . ?
C2 N1 H1A 123.0 . . ?
N1 C2 H2 129.2 . . ?
N2 C2 N1 102(4) . . ?
N2 C2 H2 129.2 . . ?
C3 N2 C2 116(9) . . ?
C3 N2 H2A 124.0 . . ?
C2 N2 H2A 120.0 . . ?
C5 C6 H6 125.0 . . ?
C5 C6 N3 105(11) . . ?
N3 C6 H6 130.0 . . ?
C6 C5 H5 124.0 . . ?
C6 C5 N4 108.1 . . ?
N4 C5 H5 127.0 . . ?
C5 N4 H4 125.1 . . ?
C4 N4 C5 109.8 . . ?
C4 N4 H4 124.0 . . ?
N4 C4 H4A 129.0 . . ?
N4 C4 N3 105.0 . . ?
N3 C4 H4A 125.0 . . ?
C6 N3 H3A 123.0 . . ?
C4 N3 C6 111.0 . . ?
C4 N3 H3A 124.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 C1 N1 C2 1(4) . . . . ?
C1 C3 N2 C2 5(9) . . . . ?
C1 N1 C2 N2 2(4) . . . . ?
N1 C2 N2 C3 -4(8) . . . . ?
N2 C3 C1 N1 -3(7) . . . . ?
C6 C5 N4 C4 -2(15) . . . . ?
C5 C6 N3 C4 0.0 . . . . ?
C5 N4 C4 N3 0.0 . . . . ?
N4 C4 N3 C6 0.0 . . . . ?
N3 C6 C5 N4 2(13) . . . . ?

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

data_im3pbbr5_392gpa
_database_code_depnum_ccdc_archive 'CCDC 2473986'
loop_
_audit_author_name
_audit_author_address
'Kinga Roszak'
;Adam Mickiewicz University Poznan
Poland
;
_audit_update_record             
;
2025-07-18 deposited with the CCDC.	2026-03-26 downloaded from the CCDC.
;
_audit_creation_date             2025-04-14
# start Validation Reply Form
_vrf_PLAT029_im3pbbr5_392gpa     
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.242 Why?  
RESPONSE: The data come from high-pressure studies and are 
limited by the DAC opening angle.
;
_vrf_PLAT090_im3pbbr5_392gpa     
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       2.28 Note  
RESPONSE:  The data/parameter ratio is affected by the access limits of the DAC.
;
_vrf_PLAT342_im3pbbr5_392gpa     
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............        0.1 Ang.  
RESPONSE: Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the X-ray 
radiation to the measured sample
;
_vrf_PLAT911_im3pbbr5_392gpa     
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        845 Report
RESPONSE: These reflections were probably affected 
by unexpected deviations in their intensities for symmetry 
equivalent measurements and omitted during initial data reduction.
;
_vrf_PLAT915_im3pbbr5_392gpa     
;
PROBLEM: No Flack x Check Done: Low Friedel Pair Coverage         21 %     
RESPONSE: Because the Friedel Pair Coverage was low the absolute configuration was
assigned using the known absolute configuration of the molecules
;
_vrf_PLAT987_im3pbbr5_392gpa     
;
PROBLEM: The Flack x is >> 0 -  Do a BASF/TWIN Refinement     Please Check 
RESPONSE: As indicated by the Flack
parameter, the structures were refined as twins. 
All refinements converged to the racemic-twin compounds.
;
# end Validation Reply Form
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br5 Pb, 3(C3 H5 N2)'
_chemical_formula_sum            'C9 H15 Br5 N6 Pb'
_chemical_formula_weight         814.01
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   5.8103(6)
_cell_length_b                   9.030(2)
_cell_length_c                   8.837(3)
_cell_angle_alpha                65.33(3)
_cell_angle_beta                 83.145(19)
_cell_angle_gamma                85.946(17)
_cell_volume                     418.21(19)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    1015
_cell_measurement_pressure       3920000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.3680
_cell_measurement_theta_min      4.3570
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    22.030
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.24051
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.89a (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_density_diffrn    3.232
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             368
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0528
_diffrn_reflns_av_unetI/netI     0.0646
_diffrn_reflns_Laue_measured_fraction_full 0.238
_diffrn_reflns_Laue_measured_fraction_max 0.217
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            2091
_diffrn_reflns_point_group_measured_fraction_full 0.238
_diffrn_reflns_point_group_measured_fraction_max 0.217
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.583
_diffrn_reflns_theta_min         4.553
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2413
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.242
_diffrn_measured_fraction_theta_max 0.221
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  19.75   0.75   30.00   0.00 -30.00   0.00    --    73
  2  φ    140.00 200.00   0.75   30.00   0.00 -30.00   0.00    --    80
  3  φ    160.00 217.00   0.75   30.00   0.00  30.00   0.00    --    76
  4  φ    -20.00  34.75   0.75   30.00   0.00  30.00   0.00    --    73
  5  ω    -24.00  24.00   0.75   30.00    --   30.00  39.46 -12.90   64
  6  ω    -24.00  24.00   0.75   30.00    --   30.00  39.46 167.10   64
  7  ω    -50.00  10.00   0.75   30.00    --  -30.00  39.46 167.10   80
  8  ω    -50.00  10.00   0.75   30.00    --  -30.00  39.46 -12.90   80
  9  ω    -64.00  -8.50   0.75   30.00    --  -30.00  81.40 -28.90   74
 10  ω    -64.00  -8.50   0.75   30.00    --  -30.00  81.40 151.10   74
 11  ω    -19.00   8.00   0.75   30.00    --   30.00  81.40 151.10   36
 12  ω    -19.00   8.00   0.75   30.00    --   30.00  81.40 -28.90   36
 13  ω    -43.00 -21.25   0.75   30.00    --   30.00 134.60 -56.90   29
 14  ω    -43.00 -21.25   0.75   30.00    --   30.00 134.60 123.10   29
 15  ω    -90.00 -36.00   0.75   30.00    --  -30.00 134.60 123.10   72
 16  ω    -90.00 -36.00   0.75   30.00    --  -30.00 134.60 -56.90   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_axis[1]    matrixX
_diffrn_orient_matrix_axis[2]    matrixY
_diffrn_orient_matrix_axis[3]    matrixZ
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0149908895
_diffrn_orient_matrix_UB_12      -0.0443066419
_diffrn_orient_matrix_UB_13      0.0881383973
_diffrn_orient_matrix_UB_21      -0.1217931409
_diffrn_orient_matrix_UB_22      0.0124279115
_diffrn_orient_matrix_UB_23      -0.0012655040
_diffrn_orient_matrix_UB_31      -0.0082403840
_diffrn_orient_matrix_UB_32      -0.0731823992
_diffrn_orient_matrix_UB_33      -0.0103185712
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.238
_reflns_Friedel_fraction_max     0.217
_reflns_number_gt                657
_reflns_number_total             737
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXD  (Sheldrick, 2008)'
_refine_diff_density_max         0.457
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.108
_refine_ls_abs_structure_details 
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack   0.5
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         737
_refine_ls_number_restraints     245
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0389
_refine_ls_restrained_S_all      0.877
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0448P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0776
_refine_ls_wR_factor_ref         0.0805
_refine_special_details          
;
 Refined as a 2-component perfect inversion twin.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 C5-C4
 1.28 with sigma of 0.02
 C9-C8
 2.1 with sigma of 0.02
3. Rigid bond restraints
 N3, C6, N4, C5, C4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N2, C1, N1, C2, C3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N6, C9, N5, C8, C7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Br3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Br5, Br2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C5 \\sim N4 \\sim N3 \\sim C6 \\sim C4: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
C3 \\sim C2 \\sim N1 \\sim C1 \\sim N2: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
C9 \\sim N5 \\sim C8 \\sim C7 \\sim N6: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Br3: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Br2 \\sim Br5: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
Uanis(C9) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C7) \\sim
Ueq, Uanis(N6) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of
0.008
Uanis(C5) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C6) \\sim
Ueq, Uanis(N4) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of
0.008
Uanis(C3) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C1) \\sim
Ueq, Uanis(N2) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of
0.008
Uanis(Br3) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(Br5) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(Br2) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(Br1) \\sim Ueq, Uanis(Br4) \\sim Ueq: with sigma of 0.004 and sigma for
terminal atoms of 0.008
5.a :
 C3(N2,C1,N1,C2), N3(C6,N4,C5,C4), C9(N5,C8,C7,N6)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), N2(H2), C1(H1), N1(H1A), C2(H2A), N3(H3A), C6(H6), N4(H4), C5(H5),
 C4(H4A), C9(H9), N5(H5A), C8(H8), C7(H7), N6(H6A)
;
_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 1.50547(19) 0.5069(2) -0.0150(4) 0.047(5) Uani 1 1 d . . . . .
Br1 Br 1.4719(11) 0.1720(15) 0.241(3) 0.037(6) Uani 1 1 d . U . . .
Br2 Br 1.5096(12) 0.3799(16) -0.276(3) 0.038(6) Uani 1 1 d . U . . .
Br3 Br 1.0093(10) 0.5376(12) -0.009(2) 0.024(3) Uani 1 1 d . U . . .
Br4 Br 1.4538(12) 0.6377(15) 0.244(3) 0.034(6) Uani 1 1 d . U . . .
Br5 Br 1.5084(11) 0.8452(15) -0.272(3) 0.035(6) Uani 1 1 d . U . . .
C3 C 0.857(6) -0.066(8) 0.974(16) 0.039(10) Uani 1 1 d G U . . .
H3 H 0.744826 -0.132216 0.969137 0.046 Uiso 1 1 calc R U . . .
N2 N 1.075(6) -0.107(8) 1.001(16) 0.034(10) Uani 1 1 d G U . . .
H2 H 1.138011 -0.200980 1.016636 0.041 Uiso 1 1 calc R U . . .
C1 C 1.181(6) 0.018(8) 0.999(16) 0.040(10) Uani 1 1 d G U . . .
H1 H 1.336293 0.020497 1.014522 0.048 Uiso 1 1 calc R U . . .
N1 N 1.030(7) 0.136(8) 0.971(16) 0.045(10) Uani 1 1 d G U . . .
H1A H 1.054699 0.231512 0.964104 0.054 Uiso 1 1 calc R U . . .
C2 C 0.830(6) 0.084(8) 0.956(17) 0.034(10) Uani 1 1 d G U . . .
H2A H 0.692010 0.145030 0.935528 0.041 Uiso 1 1 calc R U . . .
N3 N 1.091(6) 0.327(7) 0.494(12) 0.035(9) Uani 1 1 d G U . . .
H3A H 1.166334 0.415808 0.457098 0.042 Uiso 1 1 calc R U . . .
C6 C 0.902(6) 0.307(7) 0.445(13) 0.035(10) Uani 1 1 d G U . . .
H6 H 0.821792 0.387091 0.361950 0.042 Uiso 1 1 calc R U . . .
N4 N 0.840(6) 0.157(7) 0.529(13) 0.038(9) Uani 1 1 d G U . . .
H4 H 0.718692 0.114164 0.518667 0.046 Uiso 1 1 calc R U . . .
C5 C 0.991(7) 0.084(7) 0.631(13) 0.043(10) Uani 1 1 d DG U . . .
H5 H 0.989760 -0.025078 0.706991 0.052 Uiso 1 1 calc R U . . .
C4 C 1.146(7) 0.189(8) 0.609(12) 0.034(10) Uani 1 1 d DG U . . .
H4A H 1.275787 0.168053 0.667300 0.040 Uiso 1 1 calc R U . . .
C9 C 1.006(9) -0.351(7) 0.556(13) 0.049(11) Uani 1 1 d DG U . . .
H9 H 1.037159 -0.454088 0.636823 0.058 Uiso 1 1 calc R U . . .
N5 N 1.133(8) -0.223(8) 0.514(15) 0.052(11) Uani 1 1 d G U . . .
H5A H 1.258892 -0.218598 0.554264 0.062 Uiso 1 1 calc R U . . .
C8 C 1.033(8) -0.102(7) 0.398(14) 0.051(12) Uani 1 1 d DG U . . .
H8 H 1.084864 0.003854 0.343930 0.061 Uiso 1 1 calc R U . . .
C7 C 0.843(7) -0.156(7) 0.369(13) 0.044(11) Uani 1 1 d G U . . .
H7 H 0.740302 -0.094578 0.291380 0.053 Uiso 1 1 calc R U . . .
N6 N 0.827(6) -0.310(7) 0.467(13) 0.047(11) Uani 1 1 d G U . . .
H6A H 0.719373 -0.373029 0.472386 0.056 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 2.926(19) . ?
Pb1 Br2 2.972(16) . ?
Pb1 Br3 2.969(5) 1_655 ?
Pb1 Br3 2.873(6) . ?
Pb1 Br4 2.964(16) . ?
Pb1 Br5 2.948(19) . ?
C3 H3 0.9300 . ?
C3 N2 1.31(3) . ?
C3 C2 1.30(3) . ?
N2 H2 0.8600 . ?
N2 C1 1.32(3) . ?
C1 H1 0.9300 . ?
C1 N1 1.29(3) . ?
N1 H1A 0.8600 . ?
N1 C2 1.33(3) . ?
C2 H2A 0.9300 . ?
N3 H3A 0.8600 . ?
N3 C6 1.28(2) . ?
N3 C4 1.29(2) . ?
C6 H6 0.9300 . ?
C6 N4 1.30(2) . ?
N4 H4 0.8600 . ?
N4 C5 1.27(2) . ?
C5 H5 0.9300 . ?
C5 C4 1.29(2) . ?
C4 H4A 0.9300 . ?
C9 H9 0.9300 . ?
C9 N5 1.310(19) . ?
C9 N6 1.32(2) . ?
N5 H5A 0.8600 . ?
N5 C8 1.302(19) . ?
C8 H8 0.9300 . ?
C8 C7 1.33(2) . ?
C7 H7 0.9300 . ?
C7 N6 1.294(19) . ?
N6 H6A 0.8600 . ?

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 89.0(5) . . ?
Br1 Pb1 Br3 96.2(3) . 1_655 ?
Br1 Pb1 Br4 91.3(4) . . ?
Br1 Pb1 Br5 176.5(2) . . ?
Br3 Pb1 Br1 90.9(3) . . ?
Br3 Pb1 Br2 88.4(3) . . ?
Br3 Pb1 Br2 101.1(3) 1_655 . ?
Br3 Pb1 Br3 168.16(18) . 1_655 ?
Br3 Pb1 Br4 86.2(3) . . ?
Br3 Pb1 Br5 85.6(3) . . ?
Br4 Pb1 Br2 174.7(2) . . ?
Br4 Pb1 Br3 84.2(3) . 1_655 ?
Br5 Pb1 Br2 90.9(4) . . ?
Br5 Pb1 Br3 87.2(3) . 1_655 ?
Br5 Pb1 Br4 88.5(5) . . ?
Pb1 Br3 Pb1 168.16(18) . 1_455 ?
N2 C3 H3 126.7 . . ?
C2 C3 H3 126.7 . . ?
C2 C3 N2 106.6 . . ?
C3 N2 H2 125.3 . . ?
C3 N2 C1 109.4 . . ?
C1 N2 H2 125.3 . . ?
N2 C1 H1 126.5 . . ?
N1 C1 N2 107.1 . . ?
N1 C1 H1 126.5 . . ?
C1 N1 H1A 125.9 . . ?
C1 N1 C2 108.1 . . ?
C2 N1 H1A 125.9 . . ?
C3 C2 N1 108.8 . . ?
C3 C2 H2A 125.6 . . ?
N1 C2 H2A 125.6 . . ?
C6 N3 H3A 126.6 . . ?
C6 N3 C4 106.8 . . ?
C4 N3 H3A 126.6 . . ?
N3 C6 H6 125.6 . . ?
N3 C6 N4 108.7 . . ?
N4 C6 H6 125.6 . . ?
C6 N4 H4 126.0 . . ?
C5 N4 C6 108.0 . . ?
C5 N4 H4 126.0 . . ?
N4 C5 H5 126.4 . . ?
N4 C5 C4 107.2 . . ?
C4 C5 H5 126.4 . . ?
N3 C4 C5 109.2 . . ?
N3 C4 H4A 125.4 . . ?
C5 C4 H4A 125.4 . . ?
N5 C9 H9 125.3 . . ?
N5 C9 N6 109.3 . . ?
N6 C9 H9 125.3 . . ?
C9 N5 H5A 126.7 . . ?
C8 N5 C9 106.6 . . ?
C8 N5 H5A 126.7 . . ?
N5 C8 H8 125.5 . . ?
N5 C8 C7 108.9 . . ?
C7 C8 H8 125.5 . . ?
C8 C7 H7 126.1 . . ?
N6 C7 C8 107.9 . . ?
N6 C7 H7 126.1 . . ?
C9 N6 H6A 126.4 . . ?
C7 N6 C9 107.3 . . ?
C7 N6 H6A 126.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 N2 C1 N1 0.0 . . . . ?
N2 C3 C2 N1 0.0 . . . . ?
N2 C1 N1 C2 0.0 . . . . ?
C1 N1 C2 C3 0.0 . . . . ?
C2 C3 N2 C1 0.0 . . . . ?
N3 C6 N4 C5 0.0 . . . . ?
C6 N3 C4 C5 0.0 . . . . ?
C6 N4 C5 C4 0.0 . . . . ?
N4 C5 C4 N3 0.0 . . . . ?
C4 N3 C6 N4 0.0 . . . . ?
C9 N5 C8 C7 0.0 . . . . ?
N5 C9 N6 C7 0.0 . . . . ?
N5 C8 C7 N6 0.0 . . . . ?
C8 C7 N6 C9 0.0 . . . . ?
N6 C9 N5 C8 0.0 . . . . ?

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

data_im3pbbr5_345gpa
_database_code_depnum_ccdc_archive 'CCDC 2473985'
loop_
_audit_author_name
_audit_author_address
'Kinga Roszak'
;Adam Mickiewicz University Poznan
Poland
;
_audit_update_record             
;
2025-07-18 deposited with the CCDC.	2026-03-26 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_im3pbbr5_345gpa     
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.242 Why?  
RESPONSE: The data come from high-pressure studies and are 
limited by the DAC opening angle.
;
_vrf_PLAT031_im3pbbr5_345gpa     
;
PROBLEM: Refined Extinction Parameter Within Range of ...      0.368 Sigma 
RESPONSE: Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the X-ray 
radiation to the measured sample
;
_vrf_PLAT090_im3pbbr5_345gpa     
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       2.31 Note  
RESPONSE:  The data/parameter ratio is affected by the access limits of the DAC.
;
_vrf_PLAT342_im3pbbr5_345gpa     
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............        0.1 Ang.  
RESPONSE: Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the X-ray 
radiation to the measured sample
;
_vrf_PLAT910_im3pbbr5_345gpa     
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         12 Note  
RESPONSE: These reflections were probably affected 
by unexpected deviations in their intensities for symmetry 
equivalent measurements and omitted during initial data reduction.
;
_vrf_PLAT911_im3pbbr5_345gpa     
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        841 Report
RESPONSE: These reflections were probably affected 
by unexpected deviations in their intensities for symmetry 
equivalent measurements and omitted during initial data reduction.
;
_vrf_PLAT915_im3pbbr5_345gpa     
;
PROBLEM: No Flack x Check Done: Low Friedel Pair Coverage         21 %     
RESPONSE: Because the Friedel Pair Coverage was low the absolute configuration was
assigned using the known absolute configuration of the molecules
;
_vrf_PLAT987_im3pbbr5_345gpa     
;
PROBLEM: The Flack x is >> 0 -  Do a BASF/TWIN Refinement     Please Check 
RESPONSE: As indicated by the Flack
parameter, the structures were refined as twins. 
All refinements converged to the racemic-twin compounds.
;
# end Validation Reply Form
_audit_creation_date             2025-04-14
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br5 Pb, 3(C3 H5 N2)'
_chemical_formula_sum            'C9 H15 Br5 N6 Pb'
_chemical_formula_weight         814.01
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   5.8206(4)
_cell_length_b                   9.0421(18)
_cell_length_c                   8.859(3)
_cell_angle_alpha                65.34(2)
_cell_angle_beta                 83.175(14)
_cell_angle_gamma                86.025(12)
_cell_volume                     420.62(17)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    1153
_cell_measurement_pressure       3450000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.6550
_cell_measurement_theta_min      5.4310
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    21.904
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.20139
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.89a (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_density_diffrn    3.214
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             368
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_unetI/netI     0.0549
_diffrn_reflns_Laue_measured_fraction_full 0.241
_diffrn_reflns_Laue_measured_fraction_max 0.225
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            2147
_diffrn_reflns_point_group_measured_fraction_full 0.241
_diffrn_reflns_point_group_measured_fraction_max 0.225
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.399
_diffrn_reflns_theta_min         4.693
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2413
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.242
_diffrn_measured_fraction_theta_max 0.225
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  19.75   0.75   30.00   0.00 -30.00   0.00    --    73
  2  φ    140.00 200.00   0.75   30.00   0.00 -30.00   0.00    --    80
  3  φ    160.00 217.00   0.75   30.00   0.00  30.00   0.00    --    76
  4  φ    -20.00  34.75   0.75   30.00   0.00  30.00   0.00    --    73
  5  ω    -24.00  24.00   0.75   30.00    --   30.00  39.46 -12.90   64
  6  ω    -24.00  24.00   0.75   30.00    --   30.00  39.46 167.10   64
  7  ω    -50.00  10.00   0.75   30.00    --  -30.00  39.46 167.10   80
  8  ω    -50.00  10.00   0.75   30.00    --  -30.00  39.46 -12.90   80
  9  ω    -64.00  -8.50   0.75   30.00    --  -30.00  81.40 -28.90   74
 10  ω    -64.00  -8.50   0.75   30.00    --  -30.00  81.40 151.10   74
 11  ω    -19.00   8.00   0.75   30.00    --   30.00  81.40 151.10   36
 12  ω    -19.00   8.00   0.75   30.00    --   30.00  81.40 -28.90   36
 13  ω    -43.00 -21.25   0.75   30.00    --   30.00 134.60 -56.90   29
 14  ω    -43.00 -21.25   0.75   30.00    --   30.00 134.60 123.10   29
 15  ω    -90.00 -36.00   0.75   30.00    --  -30.00 134.60 123.10   72
 16  ω    -90.00 -36.00   0.75   30.00    --  -30.00 134.60 -56.90   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_axis[1]    matrixX
_diffrn_orient_matrix_axis[2]    matrixY
_diffrn_orient_matrix_axis[3]    matrixZ
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0148351040
_diffrn_orient_matrix_UB_12      -0.0446954331
_diffrn_orient_matrix_UB_13      0.0879737123
_diffrn_orient_matrix_UB_21      -0.1214851180
_diffrn_orient_matrix_UB_22      0.0130765728
_diffrn_orient_matrix_UB_23      -0.0010118624
_diffrn_orient_matrix_UB_31      -0.0095421804
_diffrn_orient_matrix_UB_32      -0.0727008631
_diffrn_orient_matrix_UB_33      -0.0108004462
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.241
_reflns_Friedel_fraction_max     0.225
_reflns_number_gt                699
_reflns_number_total             752
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXD  (Sheldrick, 2008)'
_refine_diff_density_max         0.463
_refine_diff_density_min         -0.376
_refine_diff_density_rms         0.110
_refine_ls_abs_structure_details 
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack   0.5
_refine_ls_extinction_coef       0.0007(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         752
_refine_ls_number_restraints     245
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0364
_refine_ls_restrained_S_all      0.914
_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)+(0.0459P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0778
_refine_ls_wR_factor_ref         0.0795
_refine_special_details          
;
 Refined as a 2-component perfect inversion twin.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 C5-C4
 1.28 with sigma of 0.02
 C9-C8
 2.1 with sigma of 0.02
3. Rigid bond restraints
 N3, C6, N4, C5, C4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N2, C1, N1, C2, C3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N6, C9, N5, C8, C7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Br3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Br5, Br2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C5 \\sim N4 \\sim N3 \\sim C6 \\sim C4: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
C3 \\sim C2 \\sim N1 \\sim C1 \\sim N2: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
C9 \\sim N5 \\sim C8 \\sim C7 \\sim N6: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Br3: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Br2 \\sim Br5: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
Uanis(C9) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C7) \\sim
Ueq, Uanis(N6) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of
0.008
Uanis(C5) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C6) \\sim
Ueq, Uanis(N4) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of
0.008
Uanis(C3) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C1) \\sim
Ueq, Uanis(N2) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of
0.008
Uanis(Br3) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(Br5) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(Br2) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(Br1) \\sim Ueq, Uanis(Br4) \\sim Ueq: with sigma of 0.004 and sigma for
terminal atoms of 0.008
5.a :
 C3(N2,C1,N1,C2), N3(C6,N4,C5,C4), C9(N5,C8,C7,N6)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), N2(H2), C1(H1), N1(H1A), C2(H2A), N3(H3A), C6(H6), N4(H4), C5(H5),
 C4(H4A), C9(H9), N5(H5A), C8(H8), C7(H7), N6(H6A)
;
_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 1.50440(13) 0.50720(14) -0.0150(2) 0.031(4) Uani 1 1 d . . . . .
Br1 Br 1.4720(11) 0.1714(15) 0.242(3) 0.037(6) Uani 1 1 d . U . . .
Br2 Br 1.5106(11) 0.3790(16) -0.275(3) 0.034(6) Uani 1 1 d . U . . .
Br3 Br 1.0078(9) 0.5376(12) -0.011(2) 0.022(3) Uani 1 1 d . U . . .
Br4 Br 1.4535(11) 0.6364(14) 0.246(3) 0.031(5) Uani 1 1 d . U . . .
Br5 Br 1.5078(11) 0.8451(15) -0.271(3) 0.032(5) Uani 1 1 d . U . . .
C3 C 0.857(6) -0.066(8) 0.976(16) 0.037(10) Uani 1 1 d G U . . .
H3 H 0.742960 -0.130185 0.969965 0.044 Uiso 1 1 calc R U . . .
N2 N 1.072(6) -0.109(7) 1.005(14) 0.030(9) Uani 1 1 d G U . . .
H2 H 1.133149 -0.203706 1.022101 0.036 Uiso 1 1 calc R U . . .
C1 C 1.182(6) 0.015(8) 1.003(15) 0.038(10) Uani 1 1 d G U . . .
H1 H 1.336034 0.015606 1.020225 0.046 Uiso 1 1 calc R U . . .
N1 N 1.033(7) 0.135(8) 0.973(15) 0.046(10) Uani 1 1 d G U . . .
H1A H 1.060445 0.230147 0.965221 0.056 Uiso 1 1 calc R U . . .
C2 C 0.832(6) 0.085(8) 0.956(16) 0.035(9) Uani 1 1 d G U . . .
H2A H 0.696896 0.147947 0.933582 0.043 Uiso 1 1 calc R U . . .
N3 N 1.094(6) 0.333(7) 0.484(13) 0.040(9) Uani 1 1 d G U . . .
H3A H 1.168842 0.421639 0.445420 0.048 Uiso 1 1 calc R U . . .
C6 C 0.898(6) 0.313(7) 0.444(13) 0.038(10) Uani 1 1 d G U . . .
H6 H 0.810917 0.393803 0.367413 0.046 Uiso 1 1 calc R U . . .
N4 N 0.840(6) 0.162(7) 0.528(13) 0.039(9) Uani 1 1 d G U . . .
H4 H 0.715567 0.119633 0.522326 0.047 Uiso 1 1 calc R U . . .
C5 C 1.001(7) 0.088(7) 0.620(13) 0.045(10) Uani 1 1 d DG U . . .
H5 H 1.004332 -0.021178 0.692924 0.054 Uiso 1 1 calc R U . . .
C4 C 1.157(8) 0.194(8) 0.593(13) 0.043(10) Uani 1 1 d DG U . . .
H4A H 1.293969 0.172161 0.643446 0.052 Uiso 1 1 calc R U . . .
C9 C 1.008(8) -0.356(7) 0.569(12) 0.044(10) Uani 1 1 d DG U . . .
H9 H 1.036705 -0.458151 0.652334 0.052 Uiso 1 1 calc R U . . .
N5 N 1.136(7) -0.228(8) 0.524(14) 0.046(10) Uani 1 1 d G U . . .
H5A H 1.258856 -0.222337 0.566569 0.055 Uiso 1 1 calc R U . . .
C8 C 1.039(7) -0.110(7) 0.404(13) 0.042(11) Uani 1 1 d DG U . . .
H8 H 1.092444 -0.003994 0.348143 0.051 Uiso 1 1 calc R U . . .
C7 C 0.852(7) -0.165(7) 0.374(12) 0.042(10) Uani 1 1 d G U . . .
H7 H 0.752389 -0.105438 0.293566 0.051 Uiso 1 1 calc R U . . .
N6 N 0.833(6) -0.317(7) 0.476(12) 0.044(10) Uani 1 1 d G U . . .
H6A H 0.726441 -0.381501 0.481531 0.052 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 2.942(18) . ?
Pb1 Br2 2.972(16) . ?
Pb1 Br3 2.882(5) . ?
Pb1 Br3 2.968(5) 1_655 ?
Pb1 Br4 2.971(15) . ?
Pb1 Br5 2.948(19) . ?
C3 H3 0.9300 . ?
C3 N2 1.31(3) . ?
C3 C2 1.30(2) . ?
N2 H2 0.8600 . ?
N2 C1 1.32(3) . ?
C1 H1 0.9300 . ?
C1 N1 1.30(2) . ?
N1 H1A 0.8600 . ?
N1 C2 1.33(3) . ?
C2 H2A 0.9300 . ?
N3 H3A 0.8600 . ?
N3 C6 1.28(2) . ?
N3 C4 1.29(2) . ?
C6 H6 0.9300 . ?
C6 N4 1.30(3) . ?
N4 H4 0.8600 . ?
N4 C5 1.27(2) . ?
C5 H5 0.9300 . ?
C5 C4 1.29(3) . ?
C4 H4A 0.9300 . ?
C9 H9 0.9300 . ?
C9 N5 1.312(19) . ?
C9 N6 1.324(19) . ?
N5 H5A 0.8600 . ?
N5 C8 1.306(19) . ?
C8 H8 0.9300 . ?
C8 C7 1.329(19) . ?
C7 H7 0.9300 . ?
C7 N6 1.298(19) . ?
N6 H6A 0.8600 . ?

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 89.0(5) . . ?
Br1 Pb1 Br3 96.0(3) . 1_655 ?
Br1 Pb1 Br4 90.8(4) . . ?
Br1 Pb1 Br5 176.7(2) . . ?
Br3 Pb1 Br1 91.1(3) . . ?
Br3 Pb1 Br2 88.4(3) . . ?
Br3 Pb1 Br2 100.6(3) 1_655 . ?
Br3 Pb1 Br3 168.55(16) . 1_655 ?
Br3 Pb1 Br4 84.4(3) 1_655 . ?
Br3 Pb1 Br4 86.6(3) . . ?
Br3 Pb1 Br5 85.6(3) . . ?
Br4 Pb1 Br2 175.0(2) . . ?
Br5 Pb1 Br2 91.1(4) . . ?
Br5 Pb1 Br3 87.2(3) . 1_655 ?
Br5 Pb1 Br4 88.8(5) . . ?
Pb1 Br3 Pb1 168.55(16) . 1_455 ?
N2 C3 H3 126.7 . . ?
C2 C3 H3 126.7 . . ?
C2 C3 N2 106.7 . . ?
C3 N2 H2 125.3 . . ?
C3 N2 C1 109.4 . . ?
C1 N2 H2 125.3 . . ?
N2 C1 H1 126.5 . . ?
N1 C1 N2 107.1 . . ?
N1 C1 H1 126.5 . . ?
C1 N1 H1A 125.9 . . ?
C1 N1 C2 108.1 . . ?
C2 N1 H1A 125.9 . . ?
C3 C2 N1 108.7 . . ?
C3 C2 H2A 125.6 . . ?
N1 C2 H2A 125.6 . . ?
C6 N3 H3A 126.6 . . ?
C6 N3 C4 106.9 . . ?
C4 N3 H3A 126.6 . . ?
N3 C6 H6 125.6 . . ?
N3 C6 N4 108.7 . . ?
N4 C6 H6 125.6 . . ?
C6 N4 H4 126.0 . . ?
C5 N4 C6 108.0 . . ?
C5 N4 H4 126.0 . . ?
N4 C5 H5 126.3 . . ?
N4 C5 C4 107.3 . . ?
C4 C5 H5 126.3 . . ?
N3 C4 C5 109.1 . . ?
N3 C4 H4A 125.5 . . ?
C5 C4 H4A 125.5 . . ?
N5 C9 H9 125.4 . . ?
N5 C9 N6 109.3 . . ?
N6 C9 H9 125.4 . . ?
C9 N5 H5A 126.7 . . ?
C8 N5 C9 106.7 . . ?
C8 N5 H5A 126.7 . . ?
N5 C8 H8 125.5 . . ?
N5 C8 C7 108.9 . . ?
C7 C8 H8 125.5 . . ?
C8 C7 H7 126.1 . . ?
N6 C7 C8 107.8 . . ?
N6 C7 H7 126.1 . . ?
C9 N6 H6A 126.3 . . ?
C7 N6 C9 107.3 . . ?
C7 N6 H6A 126.3 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 N2 C1 N1 0.0 . . . . ?
N2 C3 C2 N1 0.0 . . . . ?
N2 C1 N1 C2 0.0 . . . . ?
C1 N1 C2 C3 0.0 . . . . ?
C2 C3 N2 C1 0.0 . . . . ?
N3 C6 N4 C5 0.0 . . . . ?
C6 N3 C4 C5 0.0 . . . . ?
C6 N4 C5 C4 0.0 . . . . ?
N4 C5 C4 N3 0.0 . . . . ?
C4 N3 C6 N4 0.0 . . . . ?
C9 N5 C8 C7 0.0 . . . . ?
N5 C9 N6 C7 0.0 . . . . ?
N5 C8 C7 N6 0.0 . . . . ?
C8 C7 N6 C9 0.0 . . . . ?
N6 C9 N5 C8 0.0 . . . . ?

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

data_impbbr3_165gpa
_database_code_depnum_ccdc_archive 'CCDC 2473961'
loop_
_audit_author_name
_audit_author_address
'Kinga Roszak'
;Adam Mickiewicz University Poznan
Poland
;
_audit_update_record             
;
2025-07-18 deposited with the CCDC.	2026-03-26 downloaded from the CCDC.
;
_audit_creation_date             2025-04-15
# start Validation Reply Form
_vrf_PLAT027_impbbr3_165gpa      
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      17.50 Degree
RESPONSE: A full set of data was collected, however 
the very high angle data was poor and was omitted.
Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the 
X-ray radiation to the measured sample.
;
_vrf_PLAT029_impbbr3_165gpa      
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.459 Why?  
RESPONSE: The data come from high-pressure studies and are 
limited by the DAC opening angle.
;
_vrf_PLAT342_impbbr3_165gpa      
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............      0.105 Ang.  
RESPONSE: Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the X-ray 
radiation to the measured sample; poor quality of measurement
;
_vrf_PLAT090_impbbr3_165gpa      
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       4.35 Note  
RESPONSE: The data/parameter ratio is affected by the access limits of the DAC.
;
_vrf_PLAT911_impbbr3_165gpa      
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        169 Report
RESPONSE: These reflections were probably affected 
by unexpected deviations in their intensities for symmetry 
equivalent measurements and omitted during initial data reduction.
;
_vrf_PLAT987_impbbr3_165gpa      
;
PROBLEM: The Flack x is >> 0 -  Do a BASF/TWIN Refinement     Please Check 
RESPONSE: The structure was refined as an inversion twin.
;
# end Validation Reply Form
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br3 Pb, C3 H5 N2'
_chemical_formula_sum            'C3 H5 Br3 N2 Pb'
_chemical_formula_weight         516.01
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, z'

_cell_length_a                   13.5158(6)
_cell_length_b                   8.588(3)
_cell_length_c                   14.6421(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1699.5(7)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    1925
_cell_measurement_pressure       1650000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.2380
_cell_measurement_theta_min      4.7070
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    33.882
_exptl_absorpt_correction_T_min  0.02549
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    4.033
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0972
_diffrn_reflns_av_unetI/netI     0.0948
_diffrn_reflns_Laue_measured_fraction_full 0.459
_diffrn_reflns_Laue_measured_fraction_max 0.344
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6662
_diffrn_reflns_point_group_measured_fraction_full 0.468
_diffrn_reflns_point_group_measured_fraction_max 0.348
_diffrn_reflns_theta_full        17.500
_diffrn_reflns_theta_max         26.700
_diffrn_reflns_theta_min         4.742
_diffrn_ambient_temperature      293(2)
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_detector_area_resol_mean 16.2413
_diffrn_measured_fraction_theta_full 0.459
_diffrn_measured_fraction_theta_max 0.342
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0118378553
_diffrn_orient_matrix_UB_12      -0.0804146086
_diffrn_orient_matrix_UB_13      0.0016546621
_diffrn_orient_matrix_UB_21      0.0333090286
_diffrn_orient_matrix_UB_22      -0.0099798893
_diffrn_orient_matrix_UB_23      0.0369783254
_diffrn_orient_matrix_UB_31      -0.0387829896
_diffrn_orient_matrix_UB_32      0.0159813344
_diffrn_orient_matrix_UB_33      0.0312573389
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  19.75   0.75   35.00   0.00 -30.00   0.00    --    73
  2  φ    140.00 200.00   0.75   35.00   0.00 -30.00   0.00    --    80
  3  φ    160.00 217.00   0.75   35.00   0.00  30.00   0.00    --    76
  4  φ    -20.00  34.75   0.75   35.00   0.00  30.00   0.00    --    73
  5  ω    -24.00  24.00   0.75   35.00    --   30.00  39.46 -12.90   64
  6  ω    -24.00  24.00   0.75   35.00    --   30.00  39.46 167.10   64
  7  ω    -50.00  10.00   0.75   35.00    --  -30.00  39.46 167.10   80
  8  ω    -50.00  10.00   0.75   35.00    --  -30.00  39.46 -12.90   80
  9  ω    -64.00  -8.50   0.75   35.00    --  -30.00  81.40 -28.90   74
 10  ω    -64.00  -8.50   0.75   35.00    --  -30.00  81.40 151.10   74
 11  ω    -19.00   8.00   0.75   35.00    --   30.00  81.40 151.10   36
 12  ω    -19.00   8.00   0.75   35.00    --   30.00  81.40 -28.90   36
 13  ω    -43.00 -21.25   0.75   35.00    --   30.00 134.60 -56.90   29
 14  ω    -43.00 -21.25   0.75   35.00    --   30.00 134.60 123.10   29
 15  ω    -90.00 -36.00   0.75   35.00    --  -30.00 134.60 123.10   72
 16  ω    -90.00 -36.00   0.75   35.00    --  -30.00 134.60 -56.90   72
;
_diffrn_measurement_method       'ω and φ scans'
_reflns_Friedel_coverage         0.946
_reflns_Friedel_fraction_full    0.478
_reflns_Friedel_fraction_max     0.352
_reflns_number_gt                763
_reflns_number_total             1160
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXD  (Sheldrick, 2008)'
_refine_diff_density_max         0.851
_refine_diff_density_min         -0.670
_refine_diff_density_rms         0.193
_refine_ls_abs_structure_details 
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack   0.5
_refine_ls_extinction_coef       0.00081(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   0.925
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         1160
_refine_ls_number_restraints     194
_refine_ls_R_factor_all          0.0836
_refine_ls_R_factor_gt           0.0404
_refine_ls_restrained_S_all      0.863
_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)] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0504
_refine_ls_wR_factor_ref         0.0615
_refine_special_details          
;
 Refined as a 2-component perfect inversion twin.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Rigid bond restraints
 N4, C4, N3, C6, C5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C1, N1, C3, N2, C2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Br1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Br5, Br3, Br6, Br2, Br4, Br1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Br3, Br5, Br2, Br6, Br4, Br1, Pb1, Pb2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C4 \\sim N3 \\sim C6 \\sim C5 \\sim N4: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
N1 \\sim C3 \\sim N2 \\sim C2 \\sim C1: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
C1 \\sim N1 \\sim C3 \\sim N2 \\sim C2: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Br1: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Br3 \\sim Br6 \\sim Br4 \\sim Br2 \\sim Br5 \\sim Br1: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
Br6 \\sim Br5 \\sim Br4 \\sim Br1 \\sim Br2 \\sim Br3: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(Br1) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(C4) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C5) \\sim
Ueq, Uanis(N4) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of
0.008
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C3) \\sim
Ueq, Uanis(N1) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of
0.008
Uanis(Pb2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(Br3) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(Br5) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(Br6) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4.a :
 C3(C1,N1,C2,N2), C6(C5,N4,C4,N3)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C1(H1), N1(H1A), C2(H2), N2(H2A), C6(H6), C5(H5), N4(H4), C4(H4A),
 N3(H3A)
;
_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 0.1746(4) 0.0094(14) 0.36793(8) 0.028(3) Uani 1 1 d . U . . .
Pb2 Pb 0.1744(3) 0.0092(13) 0.62625(8) 0.0238(13) Uani 1 1 d . U . . .
Br1 Br 0.2300(12) 0.283(4) 0.2591(8) 0.040(4) Uani 1 1 d . U . . .
Br2 Br 0.0626(2) 0.2036(9) 0.4968(11) 0.037(3) Uani 1 1 d . U . . .
Br3 Br -0.0006(15) 0.000(5) 0.7439(10) 0.0301(12) Uani 1 1 d . U . . .
Br4 Br 0.34028(19) 0.0533(10) 0.4946(14) 0.035(4) Uani 1 1 d . U . . .
Br5 Br 0.1216(2) -0.2509(10) 0.5004(9) 0.0372(11) Uani 1 1 d . U . . .
Br6 Br 0.2280(12) 0.291(4) 0.7369(7) 0.034(3) Uani 1 1 d . U . . .
C3 C 0.379(3) 0.639(6) 0.454(5) 0.035(8) Uani 1 1 d G U . . .
H3 H 0.414704 0.709625 0.419409 0.042 Uiso 1 1 calc R U . . .
C1 C 0.371(3) 0.640(8) 0.543(5) 0.035(8) Uani 1 1 d G U . . .
H1 H 0.400091 0.710847 0.582619 0.042 Uiso 1 1 calc R U . . .
N1 N 0.315(4) 0.524(9) 0.567(4) 0.041(8) Uani 1 1 d G U . . .
H1A H 0.298338 0.499166 0.621750 0.050 Uiso 1 1 calc R U . . .
C2 C 0.2883(13) 0.452(5) 0.493(5) 0.038(8) Uani 1 1 d G U . . .
H2 H 0.247896 0.364077 0.489873 0.046 Uiso 1 1 calc R U . . .
N2 N 0.328(4) 0.523(10) 0.423(4) 0.041(8) Uani 1 1 d G U . . .
H2A H 0.321226 0.497194 0.366560 0.049 Uiso 1 1 calc R U . . .
C6 C 0.493(4) 0.082(10) 0.307(3) 0.048(9) Uani 1 1 d G U . . .
H6 H 0.483805 0.141603 0.359302 0.057 Uiso 1 1 calc R U . . .
C5 C 0.541(3) -0.045(10) 0.300(3) 0.048(9) Uani 1 1 d G U . . .
H5 H 0.574375 -0.095378 0.346536 0.058 Uiso 1 1 calc R U . . .
N4 N 0.536(2) -0.093(9) 0.210(3) 0.046(9) Uani 1 1 d G U . . .
H4 H 0.562846 -0.176055 0.189379 0.055 Uiso 1 1 calc R U . . .
C4 C 0.484(3) 0.004(9) 0.1624(18) 0.042(9) Uani 1 1 d G U . . .
H4A H 0.468643 -0.001525 0.100557 0.050 Uiso 1 1 calc R U . . .
N3 N 0.457(3) 0.112(9) 0.222(3) 0.049(9) Uani 1 1 d G U . . .
H3A H 0.421824 0.191847 0.208641 0.059 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 2.94(3) . ?
Pb1 Br2 2.939(14) . ?
Pb1 Br3 2.973(18) 2_554 ?
Pb1 Br4 2.932(14) . ?
Pb1 Br5 3.045(15) . ?
Pb1 Br6 2.99(3) 3_544 ?
Pb2 Br1 3.04(3) 3_545 ?
Pb2 Br2 2.943(13) . ?
Pb2 Br3 2.926(18) . ?
Pb2 Br4 2.981(15) . ?
Pb2 Br5 2.981(14) . ?
Pb2 Br6 3.00(3) . ?
C3 H3 0.9300 . ?
C3 C1 1.307(17) . ?
C3 N2 1.296(17) . ?
C1 H1 0.9300 . ?
C1 N1 1.296(17) . ?
N1 H1A 0.8600 . ?
N1 C2 1.301(17) . ?
C2 H2 0.9300 . ?
C2 N2 1.304(17) . ?
N2 H2A 0.8600 . ?
C6 H6 0.9300 . ?
C6 C5 1.27(2) . ?
C6 N3 1.35(2) . ?
C5 H5 0.9300 . ?
C5 N4 1.37(2) . ?
N4 H4 0.8600 . ?
N4 C4 1.29(2) . ?
C4 H4A 0.9300 . ?
C4 N3 1.33(2) . ?
N3 H3A 0.8600 . ?

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 91.4(6) . . ?
Br1 Pb1 Br3 83.8(8) . 2_554 ?
Br1 Pb1 Br5 173.3(5) . . ?
Br1 Pb1 Br6 92.4(10) . 3_544 ?
Br2 Pb1 Br3 90.0(6) . 2_554 ?
Br2 Pb1 Br5 83.5(3) . . ?
Br2 Pb1 Br6 174.5(6) . 3_544 ?
Br3 Pb1 Br5 100.6(7) 2_554 . ?
Br3 Pb1 Br6 86.5(6) 2_554 3_544 ?
Br4 Pb1 Br1 92.6(4) . . ?
Br4 Pb1 Br2 85.1(4) . . ?
Br4 Pb1 Br3 173.8(9) . 2_554 ?
Br4 Pb1 Br5 82.6(4) . . ?
Br4 Pb1 Br6 98.7(4) . 3_544 ?
Br6 Pb1 Br5 93.0(6) 3_544 . ?
Br2 Pb2 Br1 173.5(6) . 3_545 ?
Br2 Pb2 Br4 84.1(4) . . ?
Br2 Pb2 Br5 84.5(3) . . ?
Br2 Pb2 Br6 90.8(5) . . ?
Br3 Pb2 Br1 87.1(6) . 3_545 ?
Br3 Pb2 Br2 88.9(6) . . ?
Br3 Pb2 Br4 172.7(8) . . ?
Br3 Pb2 Br5 98.6(7) . . ?
Br3 Pb2 Br6 84.2(8) . . ?
Br4 Pb2 Br1 100.1(4) . 3_545 ?
Br4 Pb2 Br5 82.8(3) . . ?
Br4 Pb2 Br6 93.7(4) . . ?
Br5 Pb2 Br1 91.1(6) . 3_545 ?
Br5 Pb2 Br6 174.5(5) . . ?
Br6 Pb2 Br1 93.8(10) . 3_545 ?
Pb1 Br1 Pb2 165.3(10) . 3_554 ?
Pb1 Br2 Pb2 80.04(16) . . ?
Pb2 Br3 Pb1 178.4(7) . 2 ?
Pb1 Br4 Pb2 79.53(8) . . ?
Pb2 Br5 Pb1 77.7(2) . . ?
Pb1 Br6 Pb2 163.6(9) 3 . ?
C1 C3 H3 125.9 . . ?
N2 C3 H3 125.9 . . ?
N2 C3 C1 108.1 . . ?
C3 C1 H1 125.9 . . ?
N1 C1 C3 108.2 . . ?
N1 C1 H1 125.9 . . ?
C1 N1 H1A 126.2 . . ?
C1 N1 C2 107.6 . . ?
C2 N1 H1A 126.2 . . ?
N1 C2 H2 125.8 . . ?
N1 C2 N2 108.5 . . ?
N2 C2 H2 125.8 . . ?
C3 N2 C2 107.6 . . ?
C3 N2 H2A 126.2 . . ?
C2 N2 H2A 126.2 . . ?
C5 C6 H6 127.3 . . ?
C5 C6 N3 105.5 . . ?
N3 C6 H6 127.3 . . ?
C6 C5 H5 125.9 . . ?
C6 C5 N4 108.1 . . ?
N4 C5 H5 125.9 . . ?
C5 N4 H4 124.7 . . ?
C4 N4 C5 110.6 . . ?
C4 N4 H4 124.7 . . ?
N4 C4 H4A 128.1 . . ?
N4 C4 N3 103.8 . . ?
N3 C4 H4A 128.1 . . ?
C6 N3 H3A 124.0 . . ?
C4 N3 C6 112.1 . . ?
C4 N3 H3A 124.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 C1 N1 C2 0.0 . . . . ?
C1 C3 N2 C2 0.0 . . . . ?
C1 N1 C2 N2 0.0 . . . . ?
N1 C2 N2 C3 0.0 . . . . ?
N2 C3 C1 N1 0.0 . . . . ?
C6 C5 N4 C4 0.0 . . . . ?
C5 C6 N3 C4 0.0 . . . . ?
C5 N4 C4 N3 0.0 . . . . ?
N4 C4 N3 C6 0.0 . . . . ?
N3 C6 C5 N4 0.0 . . . . ?

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

data_impbbr3_124gpa
_database_code_depnum_ccdc_archive 'CCDC 2473960'
loop_
_audit_author_name
_audit_author_address
'Kinga Roszak'
;Adam Mickiewicz University Poznan
Poland
;
_audit_update_record             
;
2025-07-18 deposited with the CCDC.	2026-03-26 downloaded from the CCDC.
;
_audit_creation_date             2024-07-31
# start Validation Reply Form
_vrf_PLAT027_impbbr3_124gpa      
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      15.00 Degree
RESPONSE: A full set of data was collected, however 
the very high angle data was poor and was omitted.
Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the 
X-ray radiation to the measured sample.
;
_vrf_PLAT029_impbbr3_124gpa      
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.464 Why?  
RESPONSE: The data come from high-pressure studies and are 
limited by the DAC opening angle.
;
_vrf_PLAT342_impbbr3_124gpa      
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............      0.105 Ang.  
RESPONSE: Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the X-ray 
radiation to the measured sample; poor quality of measurement
;
_vrf_PLAT090_impbbr3_124gpa      
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       4.44 Note  
RESPONSE: The data/parameter ratio is affected by the access limits of the DAC.
;
_vrf_PLAT911_impbbr3_124gpa      
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        173 Report
RESPONSE: These reflections were probably affected 
by unexpected deviations in their intensities for symmetry 
equivalent measurements and omitted during initial data reduction.
;
_vrf_PLAT987_impbbr3_124gpa      
;
PROBLEM: The Flack x is >> 0 -  Do a BASF/TWIN Refinement     Please Check 
RESPONSE: The structure was refined as an inversion twin.
;
# end Validation Reply Form
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br3 Pb, C3 H5 N2'
_chemical_formula_sum            'C3 H5 Br3 N2 Pb'
_chemical_formula_weight         516.01
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, z'

_cell_length_a                   13.6717(6)
_cell_length_b                   8.661(4)
_cell_length_c                   14.7132(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1742.1(8)
_cell_formula_units_Z            8
_cell_measurement_pressure       1240000
_cell_measurement_reflns_used    1996
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.7300
_cell_measurement_theta_min      4.6750
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    33.053
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.09160
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
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    3.935
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1066
_diffrn_reflns_av_unetI/netI     0.0879
_diffrn_reflns_Laue_measured_fraction_full 0.464
_diffrn_reflns_Laue_measured_fraction_max 0.342
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7227
_diffrn_reflns_point_group_measured_fraction_full 0.475
_diffrn_reflns_point_group_measured_fraction_max 0.345
_diffrn_reflns_theta_full        15.000
_diffrn_reflns_theta_max         26.707
_diffrn_reflns_theta_min         4.702
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.2413
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.464
_diffrn_measured_fraction_theta_max 0.342
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  19.75   0.75   35.00   0.00 -30.00   0.00    --    73
  2  φ    140.00 200.00   0.75   35.00   0.00 -30.00   0.00    --    80
  3  φ    160.00 217.00   0.75   35.00   0.00  30.00   0.00    --    76
  4  φ    -20.00  34.75   0.75   35.00   0.00  30.00   0.00    --    73
  5  ω    -24.00  24.00   0.75   35.00    --   30.00  39.46 -12.90   64
  6  ω    -24.00  24.00   0.75   35.00    --   30.00  39.46 167.10   64
  7  ω    -50.00  10.00   0.75   35.00    --  -30.00  39.46 167.10   80
  8  ω    -50.00  10.00   0.75   35.00    --  -30.00  39.46 -12.90   80
  9  ω    -64.00  -8.50   0.75   35.00    --  -30.00  81.40 -28.90   74
 10  ω    -64.00  -8.50   0.75   35.00    --  -30.00  81.40 151.10   74
 11  ω    -19.00   8.00   0.75   35.00    --   30.00  81.40 151.10   36
 12  ω    -19.00   8.00   0.75   35.00    --   30.00  81.40 -28.90   36
 13  ω    -43.00 -21.25   0.75   35.00    --   30.00 134.60 -56.90   29
 14  ω    -43.00 -21.25   0.75   35.00    --   30.00 134.60 123.10   29
 15  ω    -90.00 -36.00   0.75   35.00    --  -30.00 134.60 123.10   72
 16  ω    -90.00 -36.00   0.75   35.00    --  -30.00 134.60 -56.90   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.939
_reflns_Friedel_fraction_full    0.488
_reflns_Friedel_fraction_max     0.348
_reflns_number_gt                818
_reflns_number_total             1226
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXD  (Sheldrick, 2008)'
_refine_diff_density_max         1.227
_refine_diff_density_min         -0.897
_refine_diff_density_rms         0.183
_refine_ls_abs_structure_details 
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack   0.5
_refine_ls_extinction_coef       0.00077(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         1226
_refine_ls_number_restraints     171
_refine_ls_R_factor_all          0.0824
_refine_ls_R_factor_gt           0.0415
_refine_ls_restrained_S_all      0.941
_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)+(0.0139P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0630
_refine_ls_wR_factor_ref         0.0757
_refine_special_details          
;
 Refined as a 2-component perfect inversion twin.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Rigid bond restraints
 C1, C3, N2, C2, N1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N4, C4, N3, C6, C5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C3 \\sim N2 \\sim C2 \\sim N1 \\sim C1: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
C5 \\sim C6 \\sim N3 \\sim C4 \\sim N4: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Uanis(C5) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(N3) \\sim
Ueq, Uanis(C6) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of
0.008
Uanis(Pb2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(Br1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(Br5) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C2) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C1) \\sim
Ueq, Uanis(N1) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of
0.008
Uanis(Br4) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(Br2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4.a :
 C2(N2,C3,C1,N1), C4(N3,C6,C5,N4)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), N2(H2A), C3(H3), C1(H1), N1(H1A), C4(H4), N3(H3A), C6(H6), C5(H5),
 N4(H4A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.1739(4) 0.0107(12) 0.36709(8) 0.024(3) Uani 1 1 d . . . . .
Pb2 Pb 0.1737(4) 0.0122(12) 0.62656(8) 0.0266(14) Uani 1 1 d . U . . .
Br1 Br 0.2302(13) 0.290(4) 0.2579(7) 0.042(4) Uani 1 1 d . U . . .
Br2 Br 0.0638(2) 0.2055(10) 0.4961(10) 0.0384(11) Uani 1 1 d . U . . .
Br3 Br -0.0005(18) -0.004(4) 0.7433(11) 0.032(5) Uani 1 1 d . . . . .
Br4 Br 0.33800(19) 0.0539(10) 0.4902(8) 0.0299(15) Uani 1 1 d . U . . .
Br5 Br 0.1206(2) -0.2451(11) 0.4986(10) 0.0384(12) Uani 1 1 d . U . . .
Br6 Br 0.2310(13) 0.286(4) 0.7371(7) 0.038(8) Uani 1 1 d . . . . .
C2 C 0.2887(15) 0.446(5) 0.497(6) 0.046(8) Uani 1 1 d G U . . .
H2 H 0.249052 0.359053 0.498905 0.055 Uiso 1 1 calc R U . . .
N2 N 0.314(4) 0.520(10) 0.424(4) 0.045(8) Uani 1 1 d G U . . .
H2A H 0.297984 0.497477 0.369594 0.055 Uiso 1 1 calc R U . . .
C3 C 0.369(3) 0.635(8) 0.449(5) 0.043(9) Uani 1 1 d G U . . .
H3 H 0.398062 0.706589 0.410098 0.051 Uiso 1 1 calc R U . . .
C1 C 0.378(3) 0.631(6) 0.536(5) 0.042(9) Uani 1 1 d G U . . .
H1 H 0.413121 0.700436 0.571602 0.050 Uiso 1 1 calc R U . . .
N1 N 0.328(4) 0.515(10) 0.566(4) 0.047(8) Uani 1 1 d G U . . .
H1A H 0.321658 0.487778 0.622000 0.057 Uiso 1 1 calc R U . . .
C4 C 0.477(3) -0.008(9) 0.1684(19) 0.039(9) Uani 1 1 d G U . . .
H4 H 0.460643 -0.003004 0.107096 0.047 Uiso 1 1 calc R U . . .
N3 N 0.450(2) 0.091(9) 0.231(4) 0.046(9) Uani 1 1 d G U . . .
H3A H 0.414494 0.171239 0.222764 0.055 Uiso 1 1 calc R U . . .
C6 C 0.488(4) 0.046(10) 0.308(2) 0.047(9) Uani 1 1 d G U . . .
H6 H 0.480188 0.094692 0.364214 0.056 Uiso 1 1 calc R U . . .
C5 C 0.538(3) -0.081(10) 0.294(3) 0.044(9) Uani 1 1 d G U . . .
H5 H 0.571649 -0.137437 0.336956 0.052 Uiso 1 1 calc R U . . .
N4 N 0.531(3) -0.114(9) 0.207(3) 0.044(9) Uani 1 1 d G U . . .
H4A H 0.557387 -0.191527 0.180263 0.053 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br1 3.00(3) . ?
Pb1 Br2 2.953(13) . ?
Pb1 Br3 2.99(2) 2_554 ?
Pb1 Br4 2.908(9) . ?
Pb1 Br5 3.031(15) . ?
Pb1 Br6 3.02(3) 3_544 ?
Pb2 Br1 3.03(3) 3_545 ?
Pb2 Br2 2.957(13) . ?
Pb2 Br3 2.94(2) . ?
Pb2 Br4 3.033(9) . ?
Pb2 Br5 3.006(15) . ?
Pb2 Br6 2.98(3) . ?
C2 H2 0.9300 . ?
C2 N2 1.293(19) . ?
C2 N1 1.294(19) . ?
N2 H2A 0.8600 . ?
N2 C3 1.294(19) . ?
C3 H3 0.9300 . ?
C3 C1 1.293(19) . ?
C1 H1 0.9300 . ?
C1 N1 1.294(19) . ?
N1 H1A 0.8600 . ?
C4 H4 0.9300 . ?
C4 N3 1.31(2) . ?
C4 N4 1.31(2) . ?
N3 H3A 0.8600 . ?
N3 C6 1.31(2) . ?
C6 H6 0.9300 . ?
C6 C5 1.31(2) . ?
C5 H5 0.9300 . ?
C5 N4 1.31(2) . ?
N4 H4A 0.8600 . ?

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 Br5 172.6(4) . . ?
Br1 Pb1 Br6 94.0(8) . 3_544 ?
Br2 Pb1 Br1 90.8(5) . . ?
Br2 Pb1 Br3 90.0(6) . 2_554 ?
Br2 Pb1 Br5 83.4(3) . . ?
Br2 Pb1 Br6 173.8(6) . 3_544 ?
Br3 Pb1 Br1 83.9(7) 2_554 . ?
Br3 Pb1 Br5 100.6(6) 2_554 . ?
Br3 Pb1 Br6 86.7(7) 2_554 3_544 ?
Br4 Pb1 Br1 91.8(4) . . ?
Br4 Pb1 Br2 85.3(3) . . ?
Br4 Pb1 Br3 173.6(8) . 2_554 ?
Br4 Pb1 Br5 83.2(3) . . ?
Br4 Pb1 Br6 98.4(4) . 3_544 ?
Br6 Pb1 Br5 92.1(6) 3_544 . ?
Br1 Pb2 Br4 100.2(4) 3_545 . ?
Br2 Pb2 Br1 174.1(6) . 3_545 ?
Br2 Pb2 Br4 83.1(3) . . ?
Br2 Pb2 Br5 83.7(3) . . ?
Br2 Pb2 Br6 92.1(5) . . ?
Br3 Pb2 Br1 87.1(7) . 3_545 ?
Br3 Pb2 Br2 89.7(6) . . ?
Br3 Pb2 Br4 172.7(6) . . ?
Br3 Pb2 Br5 97.8(6) . . ?
Br3 Pb2 Br6 86.1(7) . . ?
Br5 Pb2 Br1 91.9(6) . 3_545 ?
Br5 Pb2 Br4 81.6(3) . . ?
Br6 Pb2 Br1 92.5(9) . 3_545 ?
Br6 Pb2 Br4 94.1(4) . . ?
Br6 Pb2 Br5 174.3(4) . . ?
Pb1 Br1 Pb2 164.7(8) . 3_554 ?
Pb1 Br2 Pb2 80.48(18) . . ?
Pb2 Br3 Pb1 177.7(11) . 2 ?
Pb1 Br4 Pb2 79.94(8) . . ?
Pb2 Br5 Pb1 78.5(2) . . ?
Pb2 Br6 Pb1 166.1(9) . 3 ?
N2 C2 H2 126.0 . . ?
N2 C2 N1 108.0 . . ?
N1 C2 H2 126.0 . . ?
C2 N2 H2A 126.0 . . ?
C2 N2 C3 108.0 . . ?
C3 N2 H2A 126.0 . . ?
N2 C3 H3 126.0 . . ?
C1 C3 N2 108.0 . . ?
C1 C3 H3 126.0 . . ?
C3 C1 H1 126.0 . . ?
C3 C1 N1 108.0 . . ?
N1 C1 H1 126.0 . . ?
C2 N1 H1A 126.0 . . ?
C1 N1 C2 108.0 . . ?
C1 N1 H1A 126.0 . . ?
N3 C4 H4 126.0 . . ?
N3 C4 N4 108.0 . . ?
N4 C4 H4 126.0 . . ?
C4 N3 H3A 126.0 . . ?
C4 N3 C6 108.0 . . ?
C6 N3 H3A 126.0 . . ?
N3 C6 H6 126.0 . . ?
C5 C6 N3 108.0 . . ?
C5 C6 H6 126.0 . . ?
C6 C5 H5 126.0 . . ?
N4 C5 C6 108.0 . . ?
N4 C5 H5 126.0 . . ?
C4 N4 H4A 126.0 . . ?
C5 N4 C4 108.0 . . ?
C5 N4 H4A 126.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 N2 C3 C1 0.0 . . . . ?
N2 C2 N1 C1 0.0 . . . . ?
N2 C3 C1 N1 0.0 . . . . ?
C3 C1 N1 C2 0.0 . . . . ?
N1 C2 N2 C3 0.0 . . . . ?
C4 N3 C6 C5 0.0 . . . . ?
N3 C4 N4 C5 0.0 . . . . ?
N3 C6 C5 N4 0.0 . . . . ?
C6 C5 N4 C4 0.0 . . . . ?
N4 C4 N3 C6 0.0 . . . . ?

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

data_impbbr3_265gpa
_database_code_depnum_ccdc_archive 'CCDC 2473964'
loop_
_audit_author_name
_audit_author_address
'Kinga Roszak'
;Adam Mickiewicz University Poznan
Poland
;
_audit_update_record             
;
2025-07-18 deposited with the CCDC.	2026-03-26 downloaded from the CCDC.
;
_audit_creation_date             2024-08-01
# start Validation Reply Form
_vrf_PLAT027_impbbr3_265gpa      
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      17.50 Degree
RESPONSE: A full set of data was collected, however 
the very high angle data was poor and was omitted.
Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the 
X-ray radiation to the measured sample.
;
_vrf_PLAT029_impbbr3_265gpa      
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.504 Why?  
RESPONSE: The data come from high-pressure studies and are 
limited by the DAC opening angle.
;
_vrf_PLAT090_impbbr3_265gpa      
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       4.41 Note  
RESPONSE: The data/parameter ratio is affected by the access limits of the DAC.
;
_vrf_PLAT342_impbbr3_265gpa      
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............      0.065 Ang.  
RESPONSE: Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the X-ray 
radiation to the measured sample; poor quality of measurement
;
_vrf_PLAT911_impbbr3_265gpa      
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        329 Report
RESPONSE: These reflections were probably affected 
by unexpected deviations in their intensities for symmetry 
equivalent measurements and omitted during initial data reduction.
;
_vrf_PLAT987_impbbr3_265gpa      
;
PROBLEM: The Flack x is >> 0 -  Do a BASF/TWIN Refinement     Please Check 
RESPONSE: The structure was refined as an inversion twin.
;
# end Validation Reply Form
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br3 Pb, C3 H5 N2'
_chemical_formula_sum            'C3 H5 Br3 N2 Pb'
_chemical_formula_weight         516.01
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z+1/2'

_cell_length_a                   13.2728(8)
_cell_length_b                   8.449(4)
_cell_length_c                   14.5088(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1627.1(7)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    1969
_cell_measurement_pressure       2650000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.5460
_cell_measurement_theta_min      4.7820
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    35.390
_exptl_absorpt_correction_T_min  0.28287
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    4.213
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0787
_diffrn_reflns_av_unetI/netI     0.0707
_diffrn_reflns_Laue_measured_fraction_full 0.504
_diffrn_reflns_Laue_measured_fraction_max 0.362
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7077
_diffrn_reflns_point_group_measured_fraction_full 0.512
_diffrn_reflns_point_group_measured_fraction_max 0.365
_diffrn_reflns_theta_full        17.500
_diffrn_reflns_theta_max         26.750
_diffrn_reflns_theta_min         4.812
_diffrn_ambient_temperature      293(2)
_diffrn_ambient_environment      air
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_detector_area_resol_mean 16.2413
_diffrn_measured_fraction_theta_full 0.504
_diffrn_measured_fraction_theta_max 0.362
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0142546730
_diffrn_orient_matrix_UB_12      -0.0808617006
_diffrn_orient_matrix_UB_13      0.0014181605
_diffrn_orient_matrix_UB_21      0.0330551179
_diffrn_orient_matrix_UB_22      -0.0124815552
_diffrn_orient_matrix_UB_23      0.0377279798
_diffrn_orient_matrix_UB_31      -0.0394749285
_diffrn_orient_matrix_UB_32      0.0187084901
_diffrn_orient_matrix_UB_33      0.0310979847
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  19.75   0.75   35.00   0.00 -30.00   0.00    --    73
  2  φ    140.00 200.00   0.75   35.00   0.00 -30.00   0.00    --    80
  3  φ    160.00 217.00   0.75   35.00   0.00  30.00   0.00    --    76
  4  φ    -20.00  34.75   0.75   35.00   0.00  30.00   0.00    --    73
  5  ω    -24.00  24.00   0.75   35.00    --   30.00  39.46 -12.90   64
  6  ω    -24.00  24.00   0.75   35.00    --   30.00  39.46 167.10   64
  7  ω    -50.00  10.00   0.75   35.00    --  -30.00  39.46 167.10   80
  8  ω    -50.00  10.00   0.75   35.00    --  -30.00  39.46 -12.90   80
  9  ω    -64.00  -8.50   0.75   35.00    --  -30.00  81.40 -28.90   74
 10  ω    -64.00  -8.50   0.75   35.00    --  -30.00  81.40 151.10   74
 11  ω    -19.00   8.00   0.75   35.00    --   30.00  81.40 151.10   36
 12  ω    -19.00   8.00   0.75   35.00    --   30.00  81.40 -28.90   36
 13  ω    -43.00 -21.25   0.75   35.00    --   30.00 134.60 -56.90   29
 14  ω    -43.00 -21.25   0.75   35.00    --   30.00 134.60 123.10   29
 15  ω    -90.00 -36.00   0.75   35.00    --  -30.00 134.60 123.10   72
 16  ω    -90.00 -36.00   0.75   35.00    --  -30.00 134.60 -56.90   72
;
_diffrn_measurement_method       'ω and φ scans'
_reflns_Friedel_coverage         0.940
_reflns_Friedel_fraction_full    0.521
_reflns_Friedel_fraction_max     0.369
_reflns_number_gt                918
_reflns_number_total             1227
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.888
_refine_diff_density_min         -0.913
_refine_diff_density_rms         0.211
_refine_ls_abs_structure_details 
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack   0.5
_refine_ls_extinction_coef       0.00089(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         1227
_refine_ls_number_restraints     123
_refine_ls_R_factor_all          0.0685
_refine_ls_R_factor_gt           0.0406
_refine_ls_restrained_S_all      0.981
_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)+(0.0270P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0677
_refine_ls_wR_factor_ref         0.0768
_refine_special_details          
;
 Refined as a 2-component perfect inversion twin.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Rigid bond restraints
 N1, C2, N2, C3, C1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N4, C4, N3, C6, C5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C2 \\sim N2 \\sim C3 \\sim C1 \\sim N1: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
C4 \\sim N3 \\sim C6 \\sim C5 \\sim N4: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Uanis(C3) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.004 and sigma for
terminal atoms of 0.008
Uanis(C4) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C5) \\sim
Ueq, Uanis(N4) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of
0.008
4.a :
 C2(N2,C3,C1,N1), C6(C5,N4,C4,N3)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), N2(H2A), C3(H3), C1(H1), N1(H1A), C6(H6), C5(H5), N4(H4), C4(H4A),
 N3(H3A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.16934(12) -0.0013(5) 0.36828(8) 0.021(2) Uani 1 1 d . . . . .
Pb2 Pb 0.18270(11) 0.0087(5) 0.62640(8) 0.025(2) Uani 1 1 d . . . . .
Br1 Br 0.2298(3) 0.2705(17) 0.2596(4) 0.030(6) Uani 1 1 d . . . . .
Br2 Br 0.0619(2) 0.2048(11) 0.4996(5) 0.033(5) Uani 1 1 d . . . . .
Br3 Br 0.0060(4) -0.0113(17) 0.7407(4) 0.029(5) Uani 1 1 d . . . . .
Br4 Br 0.3443(3) 0.0491(11) 0.4834(4) 0.031(5) Uani 1 1 d . . . . .
Br5 Br 0.1228(2) -0.2624(12) 0.5071(4) 0.034(5) Uani 1 1 d . . . . .
Br6 Br 0.2181(3) 0.3022(17) 0.7357(3) 0.028(7) Uani 1 1 d . . . . .
C2 C 0.2907(17) 0.448(5) 0.491(3) 0.039(13) Uani 1 1 d G U . . .
H2 H 0.248723 0.359830 0.489675 0.047 Uiso 1 1 calc R U . . .
N2 N 0.326(2) 0.525(6) 0.420(3) 0.031(13) Uani 1 1 d G U . . .
H2A H 0.314493 0.502738 0.362660 0.037 Uiso 1 1 calc R U . . .
C3 C 0.3824(19) 0.642(5) 0.450(3) 0.027(9) Uani 1 1 d G U . . .
H3 H 0.416588 0.715474 0.413716 0.033 Uiso 1 1 calc R U . . .
C1 C 0.3818(19) 0.638(5) 0.541(3) 0.022(9) Uani 1 1 d G U . . .
H1 H 0.415550 0.706841 0.579770 0.026 Uiso 1 1 calc R U . . .
N1 N 0.325(2) 0.517(6) 0.566(2) 0.030(12) Uani 1 1 d G U . . .
H1A H 0.312830 0.489290 0.622175 0.037 Uiso 1 1 calc R U . . .
C6 C 0.502(3) 0.066(7) 0.3099(19) 0.033(9) Uani 1 1 d G U . . .
H6 H 0.492995 0.121134 0.364690 0.040 Uiso 1 1 calc R U . . .
C5 C 0.552(2) -0.062(7) 0.298(2) 0.041(9) Uani 1 1 d G U . . .
H5 H 0.586858 -0.117896 0.343422 0.049 Uiso 1 1 calc R U . . .
N4 N 0.546(2) -0.104(7) 0.205(2) 0.040(8) Uani 1 1 d G U . . .
H4 H 0.574063 -0.185547 0.181267 0.048 Uiso 1 1 calc R U . . .
C4 C 0.492(2) -0.001(7) 0.160(2) 0.041(9) Uani 1 1 d G U . . .
H4A H 0.476023 -0.000683 0.097453 0.049 Uiso 1 1 calc R U . . .
N3 N 0.465(2) 0.104(7) 0.225(2) 0.048(9) Uani 1 1 d G U . . .
H3A H 0.428158 0.185510 0.213783 0.057 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 2.899(12) . ?
Pb1 Br2 2.949(8) . ?
Pb1 Br3 2.976(6) 2_554 ?
Pb1 Br4 2.891(5) . ?
Pb1 Br5 3.050(9) . ?
Pb1 Br6 2.947(10) 4_544 ?
Pb2 Br1 3.023(11) 4_545 ?
Pb2 Br2 2.949(8) . ?
Pb2 Br3 2.877(6) . ?
Pb2 Br4 3.004(5) . ?
Pb2 Br5 2.980(9) . ?
Pb2 Br6 2.981(13) . ?
C2 H2 0.9300 . ?
C2 N2 1.32(2) . ?
C2 N1 1.32(2) . ?
N2 H2A 0.8600 . ?
N2 C3 1.32(2) . ?
C3 H3 0.9300 . ?
C3 C1 1.32(2) . ?
C1 H1 0.9300 . ?
C1 N1 1.32(2) . ?
N1 H1A 0.8600 . ?
C6 H6 0.9300 . ?
C6 C5 1.28(2) . ?
C6 N3 1.37(2) . ?
C5 H5 0.9300 . ?
C5 N4 1.39(2) . ?
N4 H4 0.8600 . ?
N4 C4 1.30(2) . ?
C4 H4A 0.9300 . ?
C4 N3 1.34(2) . ?
N3 H3A 0.8600 . ?

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 91.0(3) . . ?
Br1 Pb1 Br3 81.4(2) . 2_554 ?
Br1 Pb1 Br5 171.1(2) . . ?
Br1 Pb1 Br6 87.2(4) . 4_544 ?
Br2 Pb1 Br3 90.2(2) . 2_554 ?
Br2 Pb1 Br5 84.4(2) . . ?
Br3 Pb1 Br5 106.2(2) 2_554 . ?
Br4 Pb1 Br1 88.6(2) . . ?
Br4 Pb1 Br2 85.87(18) . . ?
Br4 Pb1 Br3 169.1(4) . 2_554 ?
Br4 Pb1 Br5 83.56(19) . . ?
Br4 Pb1 Br6 93.03(17) . 4_544 ?
Br6 Pb1 Br2 177.9(3) 4_544 . ?
Br6 Pb1 Br3 90.6(2) 4_544 2_554 ?
Br6 Pb1 Br5 97.2(3) 4_544 . ?
Br2 Pb2 Br1 169.0(2) . 4_545 ?
Br2 Pb2 Br4 83.88(18) . . ?
Br2 Pb2 Br5 85.7(2) . . ?
Br2 Pb2 Br6 87.2(3) . . ?
Br3 Pb2 Br1 84.6(2) . 4_545 ?
Br3 Pb2 Br2 87.1(2) . . ?
Br3 Pb2 Br4 170.7(2) . . ?
Br3 Pb2 Br5 94.1(2) . . ?
Br3 Pb2 Br6 82.6(3) . . ?
Br4 Pb2 Br1 104.08(18) . 4_545 ?
Br5 Pb2 Br1 87.8(3) . 4_545 ?
Br5 Pb2 Br4 82.88(19) . . ?
Br5 Pb2 Br6 172.3(2) . . ?
Br6 Pb2 Br1 98.8(3) . 4_545 ?
Br6 Pb2 Br4 99.2(2) . . ?
Pb1 Br1 Pb2 169.0(4) . 4_554 ?
Pb2 Br2 Pb1 78.97(19) . . ?
Pb2 Br3 Pb1 173.7(5) . 2 ?
Pb1 Br4 Pb2 78.99(10) . . ?
Pb2 Br5 Pb1 76.9(2) . . ?
Pb1 Br6 Pb2 153.6(3) 4 . ?
N2 C2 H2 126.0 . . ?
N1 C2 H2 126.0 . . ?
N1 C2 N2 108.0 . . ?
C2 N2 H2A 126.0 . . ?
C3 N2 C2 108.0 . . ?
C3 N2 H2A 126.0 . . ?
N2 C3 H3 126.0 . . ?
N2 C3 C1 108.0 . . ?
C1 C3 H3 126.0 . . ?
C3 C1 H1 126.0 . . ?
N1 C1 C3 108.0 . . ?
N1 C1 H1 126.0 . . ?
C2 N1 H1A 126.0 . . ?
C1 N1 C2 108.0 . . ?
C1 N1 H1A 126.0 . . ?
C5 C6 H6 127.4 . . ?
C5 C6 N3 105.2 . . ?
N3 C6 H6 127.4 . . ?
C6 C5 H5 126.0 . . ?
C6 C5 N4 108.1 . . ?
N4 C5 H5 126.0 . . ?
C5 N4 H4 124.6 . . ?
C4 N4 C5 110.8 . . ?
C4 N4 H4 124.6 . . ?
N4 C4 H4A 128.3 . . ?
N4 C4 N3 103.5 . . ?
N3 C4 H4A 128.3 . . ?
C6 N3 H3A 123.8 . . ?
C4 N3 C6 112.4 . . ?
C4 N3 H3A 123.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 N2 C3 C1 0.0 . . . . ?
N2 C2 N1 C1 0.0 . . . . ?
N2 C3 C1 N1 0.0 . . . . ?
C3 C1 N1 C2 0.0 . . . . ?
N1 C2 N2 C3 0.0 . . . . ?
C6 C5 N4 C4 0.0 . . . . ?
C5 C6 N3 C4 0.0 . . . . ?
C5 N4 C4 N3 0.0 . . . . ?
N4 C4 N3 C6 0.0 . . . . ?
N3 C6 C5 N4 0.0 . . . . ?

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

data_impbbr3_200gpa
_database_code_depnum_ccdc_archive 'CCDC 2473962'
loop_
_audit_author_name
_audit_author_address
'Kinga Roszak'
;Adam Mickiewicz University Poznan
Poland
;
_audit_update_record             
;
2025-07-18 deposited with the CCDC.	2026-03-26 downloaded from the CCDC.
;
_audit_creation_date             2025-04-15
# start Validation Reply Form
_vrf_PLAT027_impbbr3_200gpa      
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      15.00 Degree
RESPONSE: A full set of data was collected, however 
the very high angle data was poor and was omitted.
Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the 
X-ray radiation to the measured sample.
;
_vrf_PLAT029_impbbr3_200gpa      
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.501 Why?  
RESPONSE: The data come from high-pressure studies and are 
limited by the DAC opening angle.
;
_vrf_PLAT090_impbbr3_200gpa      
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       4.34 Note  
RESPONSE: The data/parameter ratio is affected by the access limits of the DAC.
;
_vrf_PLAT342_impbbr3_200gpa      
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............      0.085 Ang.  
RESPONSE: Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the X-ray 
radiation to the measured sample; poor quality of measurement
;
_vrf_PLAT911_impbbr3_200gpa      
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        358 Report
RESPONSE: These reflections were probably affected 
by unexpected deviations in their intensities for symmetry 
equivalent measurements and omitted during initial data reduction.
;
_vrf_PLAT987_impbbr3_200gpa      
;
PROBLEM: The Flack x is >> 0 -  Do a BASF/TWIN Refinement     Please Check 
RESPONSE: The structure was refined as an inversion twin.
;
# end Validation Reply Form
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br3 Pb, C3 H5 N2'
_chemical_formula_sum            'C3 H5 Br3 N2 Pb'
_chemical_formula_weight         516.01
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, z'

_cell_length_a                   13.4525(7)
_cell_length_b                   8.549(4)
_cell_length_c                   14.6220(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1681.6(7)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    1982
_cell_measurement_pressure       2000000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.3250
_cell_measurement_theta_min      4.7280
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    34.242
_exptl_absorpt_correction_T_min  0.41530
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    4.076
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0806
_diffrn_reflns_av_unetI/netI     0.0659
_diffrn_reflns_Laue_measured_fraction_full 0.501
_diffrn_reflns_Laue_measured_fraction_max 0.352
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7258
_diffrn_reflns_point_group_measured_fraction_full 0.511
_diffrn_reflns_point_group_measured_fraction_max 0.356
_diffrn_reflns_theta_full        15.000
_diffrn_reflns_theta_max         26.577
_diffrn_reflns_theta_min         4.759
_diffrn_ambient_temperature      293(2)
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_detector_area_resol_mean 16.2413
_diffrn_measured_fraction_theta_full 0.501
_diffrn_measured_fraction_theta_max 0.352
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0140417513
_diffrn_orient_matrix_UB_12      -0.0799107316
_diffrn_orient_matrix_UB_13      -0.0001666244
_diffrn_orient_matrix_UB_21      0.0326198975
_diffrn_orient_matrix_UB_22      -0.0144299596
_diffrn_orient_matrix_UB_23      0.0371775550
_diffrn_orient_matrix_UB_31      -0.0389922776
_diffrn_orient_matrix_UB_32      0.0167442338
_diffrn_orient_matrix_UB_33      0.0311911722
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  19.75   0.75   35.00   0.00 -30.00   0.00    --    73
  2  φ    140.00 200.00   0.75   35.00   0.00 -30.00   0.00    --    80
  3  φ    160.00 217.00   0.75   35.00   0.00  30.00   0.00    --    76
  4  φ    -20.00  34.75   0.75   35.00   0.00  30.00   0.00    --    73
  5  ω    -24.00  24.00   0.75   35.00    --   30.00  39.46 -12.90   64
  6  ω    -24.00  24.00   0.75   35.00    --   30.00  39.46 167.10   64
  7  ω    -50.00  10.00   0.75   35.00    --  -30.00  39.46 167.10   80
  8  ω    -50.00  10.00   0.75   35.00    --  -30.00  39.46 -12.90   80
  9  ω    -64.00  -8.50   0.75   35.00    --  -30.00  81.40 -28.90   74
 10  ω    -64.00  -8.50   0.75   35.00    --  -30.00  81.40 151.10   74
 11  ω    -19.00   8.00   0.75   35.00    --   30.00  81.40 151.10   36
 12  ω    -19.00   8.00   0.75   35.00    --   30.00  81.40 -28.90   36
 13  ω    -43.00 -21.25   0.75   35.00    --   30.00 134.60 -56.90   29
 14  ω    -43.00 -21.25   0.75   35.00    --   30.00 134.60 123.10   29
 15  ω    -90.00 -36.00   0.75   35.00    --  -30.00 134.60 123.10   72
 16  ω    -90.00 -36.00   0.75   35.00    --  -30.00 134.60 -56.90   72
;
_diffrn_measurement_method       'ω and φ scans'
_reflns_Friedel_coverage         0.941
_reflns_Friedel_fraction_full    0.522
_reflns_Friedel_fraction_max     0.359
_reflns_number_gt                847
_reflns_number_total             1230
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXD  (Sheldrick, 2008)'
_refine_diff_density_max         1.007
_refine_diff_density_min         -0.755
_refine_diff_density_rms         0.185
_refine_ls_abs_structure_details 
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack   0.5
_refine_ls_extinction_coef       0.00084(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         1230
_refine_ls_number_restraints     165
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0389
_refine_ls_restrained_S_all      0.986
_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)+(0.0226P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0615
_refine_ls_wR_factor_ref         0.0715
_refine_special_details          
;
 Refined as a 2-component perfect inversion twin.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Rigid bond restraints
 N4, C4, N3, C6, C5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C1, N1, C3, N2, C2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Br1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Br5, Br3, Br6, Br2, Br4, Br1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C4 \\sim N3 \\sim C6 \\sim C5 \\sim N4: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
N1 \\sim C3 \\sim N2 \\sim C2 \\sim C1: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
C1 \\sim N1 \\sim C3 \\sim N2 \\sim C2: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Br1: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Br3 \\sim Br6 \\sim Br4 \\sim Br2 \\sim Br5 \\sim Br1: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(Br1) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(C4) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C5) \\sim
Ueq, Uanis(N4) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of
0.008
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C3) \\sim
Ueq, Uanis(N1) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of
0.008
Uanis(Pb2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(Br5) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(Br3) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
4.a :
 C3(C1,N1,C2,N2), C6(C5,N4,C4,N3)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C1(H1), N1(H1A), C2(H2), N2(H2A), C6(H6), C5(H5), N4(H4), C4(H4A),
 N3(H3A)
;
_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 0.1749(4) 0.0084(12) 0.36799(8) 0.030(3) Uani 1 1 d . . . . .
Pb2 Pb 0.1748(4) 0.0090(12) 0.62605(7) 0.0233(14) Uani 1 1 d . U . . .
Br1 Br 0.2280(10) 0.284(4) 0.2596(8) 0.031(4) Uani 1 1 d . U . . .
Br2 Br 0.06191(19) 0.2032(9) 0.4972(11) 0.033(4) Uani 1 1 d . . . . .
Br3 Br -0.0003(16) -0.005(4) 0.7475(14) 0.031(2) Uani 1 1 d . U . . .
Br4 Br 0.34126(19) 0.0526(10) 0.4956(14) 0.040(4) Uani 1 1 d . . . . .
Br5 Br 0.1219(2) -0.2540(10) 0.5017(9) 0.0349(12) Uani 1 1 d . U . . .
Br6 Br 0.2281(11) 0.290(4) 0.7374(8) 0.041(7) Uani 1 1 d . . . . .
C3 C 0.377(2) 0.645(6) 0.447(4) 0.022(8) Uani 1 1 d G U . . .
H3 H 0.410717 0.718979 0.412376 0.027 Uiso 1 1 calc R U . . .
C1 C 0.380(2) 0.633(5) 0.535(4) 0.024(8) Uani 1 1 d G U . . .
H1 H 0.415944 0.696306 0.574731 0.029 Uiso 1 1 calc R U . . .
N1 N 0.325(3) 0.518(7) 0.559(2) 0.032(8) Uani 1 1 d G U . . .
H1A H 0.314265 0.485415 0.613610 0.038 Uiso 1 1 calc R U . . .
C2 C 0.2878(13) 0.459(4) 0.485(3) 0.030(8) Uani 1 1 d G U . . .
H2 H 0.244850 0.373738 0.482316 0.036 Uiso 1 1 calc R U . . .
N2 N 0.320(3) 0.537(7) 0.416(2) 0.028(8) Uani 1 1 d G U . . .
H2A H 0.306185 0.520725 0.359683 0.033 Uiso 1 1 calc R U . . .
C6 C 0.496(3) 0.062(8) 0.311(2) 0.030(8) Uani 1 1 d G U . . .
H6 H 0.488452 0.114216 0.366759 0.036 Uiso 1 1 calc R U . . .
C5 C 0.545(3) -0.063(8) 0.296(3) 0.033(8) Uani 1 1 d G U . . .
H5 H 0.581017 -0.118831 0.339610 0.039 Uiso 1 1 calc R U . . .
N4 N 0.536(2) -0.099(7) 0.205(3) 0.032(8) Uani 1 1 d G U . . .
H4 H 0.562850 -0.178864 0.179339 0.038 Uiso 1 1 calc R U . . .
C4 C 0.481(2) 0.003(8) 0.1637(16) 0.027(8) Uani 1 1 d G U . . .
H4A H 0.462613 0.005149 0.102264 0.032 Uiso 1 1 calc R U . . .
N3 N 0.456(2) 0.102(7) 0.229(3) 0.035(8) Uani 1 1 d G U . . .
H3A H 0.418805 0.182925 0.220969 0.042 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 2.93(3) . ?
Pb1 Br2 2.942(13) . ?
Pb1 Br3 2.94(2) 2_554 ?
Pb1 Br4 2.938(14) . ?
Pb1 Br5 3.060(14) . ?
Pb1 Br6 2.97(3) 3_544 ?
Pb2 Br1 3.04(2) 3_545 ?
Pb2 Br2 2.934(13) . ?
Pb2 Br3 2.95(2) . ?
Pb2 Br4 2.965(14) . ?
Pb2 Br5 2.978(14) . ?
Pb2 Br6 2.99(3) . ?
C3 H3 0.9300 . ?
C3 C1 1.292(18) . ?
C3 N2 1.278(18) . ?
C1 H1 0.9300 . ?
C1 N1 1.279(18) . ?
N1 H1A 0.8600 . ?
N1 C2 1.287(18) . ?
C2 H2 0.9300 . ?
C2 N2 1.288(18) . ?
N2 H2A 0.8600 . ?
C6 H6 0.9300 . ?
C6 C5 1.273(18) . ?
C6 N3 1.358(19) . ?
C5 H5 0.9300 . ?
C5 N4 1.38(2) . ?
N4 H4 0.8600 . ?
N4 C4 1.295(18) . ?
C4 H4A 0.9300 . ?
C4 N3 1.326(19) . ?
N3 H3A 0.8600 . ?

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 91.0(5) . . ?
Br1 Pb1 Br3 83.0(7) . 2_554 ?
Br1 Pb1 Br4 93.1(4) . . ?
Br1 Pb1 Br5 173.0(5) . . ?
Br1 Pb1 Br6 92.9(10) . 3_544 ?
Br2 Pb1 Br5 83.4(3) . . ?
Br2 Pb1 Br6 174.3(6) . 3_544 ?
Br3 Pb1 Br2 88.7(6) 2_554 . ?
Br3 Pb1 Br4 172.6(8) 2_554 . ?
Br3 Pb1 Br5 101.0(6) 2_554 . ?
Br3 Pb1 Br6 87.7(7) 2_554 3_544 ?
Br4 Pb1 Br2 85.0(3) . . ?
Br4 Pb1 Br5 82.3(4) . . ?
Br4 Pb1 Br6 98.9(3) . 3_544 ?
Br6 Pb1 Br5 93.0(7) 3_544 . ?
Br2 Pb2 Br1 173.8(5) . 3_545 ?
Br2 Pb2 Br3 89.8(6) . . ?
Br2 Pb2 Br4 84.6(4) . . ?
Br2 Pb2 Br5 84.9(3) . . ?
Br2 Pb2 Br6 91.1(6) . . ?
Br3 Pb2 Br1 86.0(6) . 3_545 ?
Br3 Pb2 Br4 174.1(8) . . ?
Br3 Pb2 Br5 98.4(6) . . ?
Br3 Pb2 Br6 84.1(7) . . ?
Br4 Pb2 Br1 99.7(4) . 3_545 ?
Br4 Pb2 Br5 83.3(3) . . ?
Br4 Pb2 Br6 93.9(4) . . ?
Br5 Pb2 Br1 91.0(6) . 3_545 ?
Br5 Pb2 Br6 175.3(6) . . ?
Br6 Pb2 Br1 93.1(10) . 3_545 ?
Pb1 Br1 Pb2 164.2(9) . 3_554 ?
Pb2 Br2 Pb1 79.91(15) . . ?
Pb1 Br3 Pb2 178.2(15) 2 . ?
Pb1 Br4 Pb2 79.45(7) . . ?
Pb2 Br5 Pb1 77.34(19) . . ?
Pb1 Br6 Pb2 163.7(10) 3 . ?
C1 C3 H3 125.9 . . ?
N2 C3 H3 125.9 . . ?
N2 C3 C1 108.2 . . ?
C3 C1 H1 125.9 . . ?
N1 C1 C3 108.2 . . ?
N1 C1 H1 125.9 . . ?
C1 N1 H1A 126.3 . . ?
C1 N1 C2 107.5 . . ?
C2 N1 H1A 126.3 . . ?
N1 C2 H2 125.7 . . ?
N1 C2 N2 108.6 . . ?
N2 C2 H2 125.7 . . ?
C3 N2 C2 107.5 . . ?
C3 N2 H2A 126.3 . . ?
C2 N2 H2A 126.3 . . ?
C5 C6 H6 127.3 . . ?
C5 C6 N3 105.4 . . ?
N3 C6 H6 127.3 . . ?
C6 C5 H5 126.0 . . ?
C6 C5 N4 108.1 . . ?
N4 C5 H5 126.0 . . ?
C5 N4 H4 124.6 . . ?
C4 N4 C5 110.7 . . ?
C4 N4 H4 124.6 . . ?
N4 C4 H4A 128.2 . . ?
N4 C4 N3 103.6 . . ?
N3 C4 H4A 128.2 . . ?
C6 N3 H3A 123.9 . . ?
C4 N3 C6 112.2 . . ?
C4 N3 H3A 123.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 C1 N1 C2 0.0 . . . . ?
C1 C3 N2 C2 0.1 . . . . ?
C1 N1 C2 N2 0.0 . . . . ?
N1 C2 N2 C3 -0.1 . . . . ?
N2 C3 C1 N1 0.0 . . . . ?
C6 C5 N4 C4 0.0 . . . . ?
C5 C6 N3 C4 0.0 . . . . ?
C5 N4 C4 N3 0.0 . . . . ?
N4 C4 N3 C6 0.0 . . . . ?
N3 C6 C5 N4 0.0 . . . . ?

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

data_im2pbbr4_0_41gpa
_database_code_depnum_ccdc_archive 'CCDC 2473968'
loop_
_audit_author_name
_audit_author_address
'Kinga Roszak'
;Adam Mickiewicz University Poznan
Poland
;
_audit_update_record             
;
2025-07-18 deposited with the CCDC.	2026-03-26 downloaded from the CCDC.
;
_audit_creation_date             2024-08-14
# start Validation Reply Form
_vrf_RINTA01_im2pbbr4_0_41gpa    
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: High factor is a result from the weak diffraction. Due to the specificity 
of the applied measuring technique and use of a diamond-anvil cell 
limiting the access of the X-ray radiation to the measured sample.
;
_vrf_PLAT027_im2pbbr4_0_41gpa    
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      17.50 Degree
RESPONSE: A full set of data was collected, however 
the very high angle data was poor and was omitted.
Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the 
X-ray radiation to the measured sample.
;
_vrf_PLAT029_im2pbbr4_0_41gpa    
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.286 Why?  
RESPONSE: The data come from high-pressure studies and are 
limited by the DAC opening angle.
;
_vrf_PLAT031_im2pbbr4_0_41gpa    
;
PROBLEM: Refined Extinction Parameter Within Range of ...      0.429 Sigma 
RESPONSE: Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the X-ray 
radiation to the measured sample
;
_vrf_PLAT088_im2pbbr4_0_41gpa    
;
PROBLEM: Poor Data / Parameter Ratio ....................       3.97 Note  
RESPONSE: The data/parameter ratio is affected by the access limits of the DAC.
;
_vrf_PLAT342_im2pbbr4_0_41gpa    
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............      0.105 Ang.  
RESPONSE: Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the X-ray 
radiation to the measured sample; poor quality of measurement
;
_vrf_PLAT020_im2pbbr4_0_41gpa    
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.204 Report
RESPONSE: High factor is a result from the weak diffraction. Due to the specificity 
of the applied measuring technique and use of a diamond-anvil cell 
limiting the access of the X-ray radiation to the measured sample.
;
_vrf_PLAT234_im2pbbr4_0_41gpa    
;
PROBLEM: Large Hirshfeld Difference Pb1      --Br1      .       0.30 Ang.  
RESPONSE: poor quality of measurement
;
_vrf_PLAT911_im2pbbr4_0_41gpa    
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.588        734 Report
RESPONSE: These reflections were probably affected 
by unexpected deviations in their intensities for symmetry 
equivalent measurements and omitted during initial data reduction.
;
# end Validation Reply Form
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br4 Pb, 2(C3 H5 N2)'
_chemical_formula_sum            'C6 H10 Br4 N4 Pb'
_chemical_formula_weight         665.01
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   6.0172(15)
_cell_length_b                   9.261(4)
_cell_length_c                   13.551(12)
_cell_angle_alpha                74.19(6)
_cell_angle_beta                 86.64(7)
_cell_angle_gamma                88.31(3)
_cell_volume                     725.3(8)
_cell_formula_units_Z            2
_cell_measurement_pressure       410000
_cell_measurement_reflns_used    547
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      2.2040
_cell_measurement_theta_min      25.1820
_shelx_estimated_absorpt_T_max   0.397
_shelx_estimated_absorpt_T_min   0.078
_exptl_absorpt_coefficient_mu    22.626
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.6900
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.89a (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    3.045
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.2036
_diffrn_reflns_av_unetI/netI     0.2712
_diffrn_reflns_Laue_measured_fraction_full 0.286
_diffrn_reflns_Laue_measured_fraction_max 0.195
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            1344
_diffrn_reflns_point_group_measured_fraction_full 0.286
_diffrn_reflns_point_group_measured_fraction_max 0.195
_diffrn_reflns_theta_full        17.500
_diffrn_reflns_theta_max         24.709
_diffrn_reflns_theta_min         2.286
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.0169
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.286
_diffrn_measured_fraction_theta_max 0.195
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -55.00 -23.50   0.75   25.00    --  -24.84  77.00 150.00   42
  2  ω    -42.00 -13.50   0.75   25.00    --  -24.84  19.00   0.00   38
  3  ω     28.00  47.50   0.75   25.00    --  -24.84-135.00-123.00   26
  4  ω    -12.00   9.00   0.75   25.00    --  -24.84 -53.00-162.00   28
  5  ω     28.00  47.50   0.75   25.00    --  -24.84-135.00  57.00   26
  6  ω    -12.00   9.00   0.75   25.00    --  -24.84 -53.00  17.00   28
  7  ω    -65.00 -21.50   0.75   25.00    --  -24.84  97.00 -35.00   58
  8  ω    -25.00  16.25   0.75   25.00    --  -24.84 -13.00-176.00   55
  9  ω    -22.00  36.50   0.75   25.00    --  -24.84 -26.00   8.00   78
 10  ω    -11.00  36.25   0.75   25.00    --   25.86 -26.00   8.00   63
 11  ω      9.00  57.00   0.75   25.00    --   25.86 -81.00-151.00   64
 12  ω   -108.00 -87.00   0.75   25.00    --  -24.84-178.00  90.00   28
 13  ω     -6.00  22.50   0.75   25.00    --  -24.84 -38.00  30.00   38
 14  ω    -74.00 -15.50   0.75   25.00    --  -24.84 114.00 135.00   78
 15  ω    -17.00  11.50   0.75   25.00    --  -24.84 -19.00   0.00   38
 16  ω     21.00  64.50   0.75   25.00    --   25.86 -97.00  35.00   58
 17  ω    -41.00 -14.00   0.75   25.00    --   25.86  19.00  30.00   36
 18  ω     72.00  93.00   0.75   25.00    --   25.86-178.00  90.00   28
 19  ω    -19.00  16.25   0.75   25.00    --   25.86  39.00 -12.00   47
 20  ω     -8.00  11.50   0.75   25.00    --   25.86  53.00 -17.00   26
 21  ω    -74.00 -15.50   0.75   25.00    --  -24.84 114.00 -45.00   78
 22  ω    -42.00  16.50   0.75   25.00    --  -24.84  19.00-180.00   78
 23  ω    -22.00  36.50   0.75   25.00    --  -24.84 -26.00   8.00   78
 24  ω    -25.00  33.50   0.75   25.00    --  -24.84 -13.00   3.00   78
 25  ω    -47.00  11.50   0.75   25.00    --  -24.84  53.00 -17.00   78
 26  ω    -53.00   5.50   0.75   25.00    --  -24.84  67.00 -23.00   78
 27  ω    -58.00   0.50   0.75   25.00    --  -24.84  81.00 -29.00   78
 28  ω      5.00  51.50   0.75   25.00    --   25.86 -38.00-180.00   62
 29  ω    -19.00  16.25   0.75   25.00    --   25.86  39.00 167.00   47
 30  ω    -34.00  24.50   0.75   25.00    --  -24.84  13.00 176.00   78
 31  ω    -42.00  16.50   0.75   25.00    --  -24.84  39.00 167.00   78
 32  ω    -47.00 -21.50   0.75   25.00    --  -24.84  53.00 162.00   34
 33  ω    -87.00 -28.50   0.75   25.00    --  -24.84 135.00 -57.00   78
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                232
_reflns_number_total             480
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.632
_refine_diff_density_min         -0.719
_refine_diff_density_rms         0.187
_refine_ls_extinction_coef       0.0003(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         480
_refine_ls_number_restraints     154
_refine_ls_R_factor_all          0.1778
_refine_ls_R_factor_gt           0.0808
_refine_ls_restrained_S_all      0.894
_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)+(0.0370P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1482
_refine_ls_wR_factor_ref         0.1949
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 C2-C1
 2.1 with sigma of 0.02
 C6-C5
 2.05 with sigma of 0.02
3. Rigid bond restraints
 N2, C3, Br2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N1, Br4, C4, N4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N2, C2, N1, C1, C3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C5, N3, C4, C6, N4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Br2 \\sim C3 \\sim N2: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C4 \\sim N4 \\sim Br4 \\sim N1: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C2 \\sim N1 \\sim C1 \\sim C3 \\sim N2: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
N4 \\sim C6 \\sim C4 \\sim N3 \\sim C5: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Uanis(N2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(Br2) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(N1) \\sim Ueq, Uanis(Br4) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(N4) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.002
Uanis(Br3) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(N3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Pb1) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(C5) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
5.a :
 C2(N2,C3,C1,N1), C4(N3,C5,N4,C6)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), N2(H2A), C3(H3), C1(H1), N1(H1A), C4(H4), N3(H3A), C5(H5), N4(H4A),
 C6(H6)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.5104(4) 0.5729(4) 0.3294(7) 0.038(3) Uani 1 1 d . U . . .
Br1 Br 0.4966(10) 0.7262(10) 0.5005(19) 0.08(3) Uani 1 1 d . . . . .
Br2 Br 0.0102(10) 0.5696(9) 0.3330(17) 0.053(6) Uani 1 1 d . U . . .
Br3 Br 0.5061(12) 0.8657(9) 0.1747(19) 0.050(5) Uani 1 1 d . U . . .
Br4 Br 0.5240(12) 0.4121(10) 0.162(2) 0.062(3) Uani 1 1 d . U . . .
C2 C 0.996(12) 0.653(7) 0.048(12) 0.11(2) Uani 1 1 d DG U . . .
H2 H 1.021502 0.570143 0.102980 0.131 Uiso 1 1 calc R U . . .
N2 N 1.129(10) 0.766(8) 0.013(14) 0.100(19) Uani 1 1 d G U . . .
H2A H 1.255249 0.776367 0.036205 0.120 Uiso 1 1 calc R U . . .
C3 C 1.037(11) 0.859(8) -0.064(14) 0.096(19) Uani 1 1 d G U . . .
H3 H 1.096468 0.949354 -0.102916 0.115 Uiso 1 1 calc R U . . .
C1 C 0.848(11) 0.805(8) -0.076(12) 0.10(2) Uani 1 1 d DG U . . .
H1 H 0.747645 0.848886 -0.125179 0.121 Uiso 1 1 calc R U . . .
N1 N 0.823(10) 0.677(7) -0.007(13) 0.101(19) Uani 1 1 d G U . . .
H1A H 0.710417 0.619119 0.001512 0.121 Uiso 1 1 calc R U . . .
C4 C 0.063(9) 0.170(4) 0.339(10) 0.043(12) Uani 1 1 d G U . . .
H4 H 0.106176 0.265776 0.339059 0.051 Uiso 1 1 calc R U . . .
N3 N -0.113(8) 0.139(4) 0.301(9) 0.042(12) Uani 1 1 d G U . . .
H3A H -0.212003 0.202456 0.272199 0.051 Uiso 1 1 calc R U . . .
C5 C -0.115(7) -0.002(5) 0.315(9) 0.042(11) Uani 1 1 d DG U . . .
H5 H -0.225310 -0.054776 0.295151 0.051 Uiso 1 1 calc R U . . .
N4 N 0.058(7) -0.058(4) 0.360(9) 0.043(12) Uani 1 1 d G U . . .
H4A H 0.094988 -0.151186 0.378298 0.051 Uiso 1 1 calc R U . . .
C6 C 0.168(8) 0.049(5) 0.375(9) 0.040(12) Uani 1 1 d DG U . . .
H6 H 0.302738 0.039321 0.406957 0.048 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br1 3.03(3) . ?
Pb1 Br1 3.083(11) 2_666 ?
Pb1 Br2 3.010(6) 1_655 ?
Pb1 Br2 3.008(6) . ?
Pb1 Br3 2.942(11) . ?
Pb1 Br4 3.03(3) . ?
C2 H2 0.9300 . ?
C2 N2 1.295(14) . ?
C2 N1 1.295(14) . ?
N2 H2A 0.8600 . ?
N2 C3 1.295(14) . ?
C3 H3 0.9300 . ?
C3 C1 1.295(14) . ?
C1 H1 0.9300 . ?
C1 N1 1.296(14) . ?
N1 H1A 0.8600 . ?
C4 H4 0.9300 . ?
C4 N3 1.269(13) . ?
C4 C6 1.268(13) . ?
N3 H3A 0.8600 . ?
N3 C5 1.267(13) . ?
C5 H5 0.9300 . ?
C5 N4 1.268(13) . ?
N4 H4A 0.8600 . ?
N4 C6 1.268(13) . ?
C6 H6 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br1 Pb1 Br1 86.6(5) . 2_666 ?
Br1 Pb1 Br4 178.6(3) . . ?
Br2 Pb1 Br1 91.4(5) . . ?
Br2 Pb1 Br1 87.8(5) 1_655 . ?
Br2 Pb1 Br1 88.9(3) 1_655 2_666 ?
Br2 Pb1 Br1 89.3(3) . 2_666 ?
Br2 Pb1 Br2 178.1(7) . 1_655 ?
Br2 Pb1 Br4 88.6(5) . . ?
Br2 Pb1 Br4 92.2(5) 1_655 . ?
Br3 Pb1 Br1 90.7(5) . . ?
Br3 Pb1 Br1 177.1(7) . 2_666 ?
Br3 Pb1 Br2 92.2(3) . 1_655 ?
Br3 Pb1 Br2 89.5(3) . . ?
Br3 Pb1 Br4 90.7(6) . . ?
Br4 Pb1 Br1 92.0(6) . 2_666 ?
Pb1 Br1 Pb1 93.4(5) . 2_666 ?
Pb1 Br2 Pb1 178.1(7) . 1_455 ?
N2 C2 H2 126.0 . . ?
N1 C2 H2 126.0 . . ?
N1 C2 N2 108.0 . . ?
C2 N2 H2A 126.0 . . ?
C3 N2 C2 108.0 . . ?
C3 N2 H2A 126.0 . . ?
N2 C3 H3 126.0 . . ?
N2 C3 C1 108.0 . . ?
C1 C3 H3 126.0 . . ?
C3 C1 H1 126.0 . . ?
C3 C1 N1 108.0 . . ?
N1 C1 H1 126.0 . . ?
C2 N1 C1 108.0 . . ?
C2 N1 H1A 126.0 . . ?
C1 N1 H1A 126.0 . . ?
N3 C4 H4 126.0 . . ?
C6 C4 H4 126.0 . . ?
C6 C4 N3 108.0 . . ?
C4 N3 H3A 126.0 . . ?
C5 N3 C4 108.0 . . ?
C5 N3 H3A 126.0 . . ?
N3 C5 H5 126.0 . . ?
N3 C5 N4 108.0 . . ?
N4 C5 H5 126.0 . . ?
C5 N4 H4A 126.0 . . ?
C6 N4 C5 108.0 . . ?
C6 N4 H4A 126.0 . . ?
C4 C6 N4 108.0 . . ?
C4 C6 H6 126.0 . . ?
N4 C6 H6 126.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 N2 C3 C1 0.0 . . . . ?
N2 C2 N1 C1 0.0 . . . . ?
N2 C3 C1 N1 0.0 . . . . ?
C3 C1 N1 C2 0.0 . . . . ?
N1 C2 N2 C3 0.0 . . . . ?
C4 N3 C5 N4 -0.1 . . . . ?
N3 C4 C6 N4 0.0 . . . . ?
N3 C5 N4 C6 0.1 . . . . ?
C5 N4 C6 C4 0.0 . . . . ?
C6 C4 N3 C5 0.0 . . . . ?

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

data_im3pbbr5_107gpa
_database_code_depnum_ccdc_archive 'CCDC 2473980'
loop_
_audit_author_name
_audit_author_address
'Kinga Roszak'
;Adam Mickiewicz University Poznan
Poland
;
_audit_update_record             
;
2025-07-18 deposited with the CCDC.	2026-03-26 downloaded from the CCDC.
;
_audit_creation_date             2023-05-30
# start Validation Reply Form
_vrf_PLAT027_im3pbbr5_107gpa     
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      17.50 Degree
RESPONSE: A full set of data was collected, however 
the very high angle data was poor and was omitted.
Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the 
X-ray radiation to the measured sample.
;
_vrf_PLAT029_im3pbbr5_107gpa     
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.315 Why?  
RESPONSE: The data come from high-pressure studies and are 
limited by the DAC opening angle.
;
_vrf_PLAT090_im3pbbr5_107gpa     
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       2.51 Note  
RESPONSE:  The data/parameter ratio is affected by the access limits of the DAC.
;
_vrf_PLAT342_im3pbbr5_107gpa     
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.13667 Ang.  
RESPONSE: Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the X-ray 
radiation to the measured sample
;
_vrf_PLAT910_im3pbbr5_107gpa     
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         16 Note  
RESPONSE: These reflections were probably affected 
by unexpected deviations in their intensities for symmetry 
equivalent measurements and omitted during initial data reduction.
;
_vrf_PLAT911_im3pbbr5_107gpa     
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        891 Report
RESPONSE: These reflections were probably affected 
by unexpected deviations in their intensities for symmetry 
equivalent measurements and omitted during initial data reduction.
;
_vrf_PLAT915_im3pbbr5_107gpa     
;
PROBLEM: No Flack x Check Done: Low Friedel Pair Coverage         21 %     
RESPONSE: Because the Friedel Pair Coverage was low the absolute configuration was
assigned using the known absolute configuration of the molecules
;
_vrf_PLAT987_im3pbbr5_107gpa     
;
PROBLEM: The Flack x is >> 0 -  Do a BASF/TWIN Refinement     Please Check 
RESPONSE: As indicated by the Flack
parameter, the structures were refined as twins. 
All refinements converged to the racemic-twin compounds.
;
# end Validation Reply Form
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br5 Pb, 3(C3 H5 N2)'
_chemical_formula_sum            'C9 H15 Br5 N6 Pb'
_chemical_formula_weight         813.97
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   5.9703(6)
_cell_length_b                   9.196(3)
_cell_length_c                   9.275(4)
_cell_angle_alpha                66.43(3)
_cell_angle_beta                 84.81(2)
_cell_angle_gamma                87.456(17)
_cell_volume                     464.8(3)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    1103
_cell_measurement_pressure       1070000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.1390
_cell_measurement_theta_min      5.2740
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    19.822
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.00998
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.908
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             368
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_Laue_measured_fraction_full 0.315
_diffrn_reflns_Laue_measured_fraction_max 0.222
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            2303
_diffrn_reflns_point_group_measured_fraction_full 0.315
_diffrn_reflns_point_group_measured_fraction_max 0.222
_diffrn_reflns_theta_full        17.500
_diffrn_reflns_theta_max         26.275
_diffrn_reflns_theta_min         5.295
_diffrn_ambient_temperature      293(2)
_diffrn_ambient_environment      air
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_detector_area_resol_mean 16.2413
_diffrn_measured_fraction_theta_full 0.315
_diffrn_measured_fraction_theta_max 0.222
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0120384000
_diffrn_orient_matrix_UB_12      -0.0427838000
_diffrn_orient_matrix_UB_13      0.0830259000
_diffrn_orient_matrix_UB_21      -0.1179685000
_diffrn_orient_matrix_UB_22      0.0130305000
_diffrn_orient_matrix_UB_23      -0.0005773000
_diffrn_orient_matrix_UB_31      -0.0130694000
_diffrn_orient_matrix_UB_32      -0.0712915000
_diffrn_orient_matrix_UB_33      -0.0106116000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  19.75   0.75   35.00   0.00 -30.00   0.00    --    73
  2  φ    140.00 200.00   0.75   35.00   0.00 -30.00   0.00    --    80
  3  φ    160.00 217.00   0.75   35.00   0.00  30.00   0.00    --    76
  4  φ    -20.00  34.75   0.75   35.00   0.00  30.00   0.00    --    73
  5  ω    -24.00  24.00   0.75   35.00    --   30.00  39.46 -12.90   64
  6  ω    -24.00  24.00   0.75   35.00    --   30.00  39.46 167.10   64
  7  ω    -50.00  10.00   0.75   35.00    --  -30.00  39.46 167.10   80
  8  ω    -50.00  10.00   0.75   35.00    --  -30.00  39.46 -12.90   80
  9  ω    -64.00  -8.50   0.75   35.00    --  -30.00  81.40 -28.90   74
 10  ω    -64.00  -8.50   0.75   35.00    --  -30.00  81.40 151.10   74
 11  ω    -19.00   8.00   0.75   35.00    --   30.00  81.40 151.10   36
 12  ω    -19.00   8.00   0.75   35.00    --   30.00  81.40 -28.90   36
 13  ω    -43.00 -21.25   0.75   35.00    --   30.00 134.60 -56.90   29
 14  ω    -43.00 -21.25   0.75   35.00    --   30.00 134.60 123.10   29
 15  ω    -90.00 -36.00   0.75   35.00    --  -30.00 134.60 123.10   72
 16  ω    -90.00 -36.00   0.75   35.00    --  -30.00 134.60 -56.90   72
;
_diffrn_measurement_method       'ω and φ scans'
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.315
_reflns_Friedel_fraction_max     0.222
_reflns_number_gt                670
_reflns_number_total             817
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXD  (Sheldrick, 2008)'
_refine_diff_density_max         0.549
_refine_diff_density_min         -0.612
_refine_diff_density_rms         0.124
_refine_ls_abs_structure_details 
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack   0.5
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         817
_refine_ls_number_restraints     249
_refine_ls_R_factor_all          0.0694
_refine_ls_R_factor_gt           0.0542
_refine_ls_restrained_S_all      0.936
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0891P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1287
_refine_ls_wR_factor_ref         0.1398
_refine_special_details          
;
 Refined as a 2-component perfect inversion twin.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Rigid bond restraints
 N5, C8, C7, N6, C9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N3, C6, N4, C5, C4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C2, N1, C1, N2, C3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C9 \\sim N6 \\sim C7 \\sim C8 \\sim N5: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
C4 \\sim C5 \\sim N4 \\sim C6 \\sim N3: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
N1 \\sim C1 \\sim N2 \\sim C3 \\sim C2: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Uanis(C9) \\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim
Ueq, Uanis(N5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C4) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(N4) \\sim
Ueq, Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C2) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(N2) \\sim
Ueq, Uanis(C3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(Br2) \\sim Ueq, Uanis(Br1) \\sim Ueq, Uanis(Br4) \\sim Ueq, Uanis(Br3)
\\sim Ueq, Uanis(Pb1) \\sim Ueq, Uanis(Br5) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
4.a :
 C3(N2,C1,N1,C2), N3(C6,N4,C5,C4), C9(N5,C8,C7,N6)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), N2(H2), C1(H1), N1(H1A), C2(H2A), N3(H3A), C6(H6), N4(H4), C5(H5),
 C4(H4A), C9(H9), N5(H5A), C8(H8), C7(H7), N6(H6A)
;
_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 1.4884(11) 0.4999(16) 0.002(3) 0.061(5) Uani 1 1 d . U . . .
Br1 Br 1.478(2) 0.166(3) 0.254(6) 0.072(13) Uani 1 1 d . U . . .
Br2 Br 1.517(2) 0.378(3) -0.260(6) 0.076(13) Uani 1 1 d . U . . .
Br3 Br 0.983(4) 0.493(5) 0.016(10) 0.069(7) Uani 1 1 d . U . . .
Br4 Br 1.467(2) 0.625(3) 0.254(6) 0.078(13) Uani 1 1 d . U . . .
Br5 Br 1.499(3) 0.830(3) -0.242(6) 0.079(13) Uani 1 1 d . U . . .
C3 C 1.019(14) -0.145(9) 1.058(18) 0.063(14) Uani 1 1 d G U . . .
H3 H 1.040187 -0.253599 1.089411 0.076 Uiso 1 1 calc R U . . .
N2 N 1.167(8) -0.042(11) 1.066(17) 0.068(14) Uani 1 1 d G U . . .
H2 H 1.297327 -0.066412 1.102203 0.082 Uiso 1 1 calc R U . . .
C1 C 1.074(13) 0.105(9) 1.008(19) 0.061(14) Uani 1 1 d G U . . .
H1 H 1.140373 0.198012 1.000526 0.073 Uiso 1 1 calc R U . . .
N1 N 0.869(10) 0.094(11) 0.964(19) 0.066(13) Uani 1 1 d G U . . .
H1A H 0.776328 0.171469 0.923403 0.079 Uiso 1 1 calc R U . . .
C2 C 0.835(11) -0.060(11) 0.994(19) 0.071(15) Uani 1 1 d G U . . .
H2A H 0.707083 -0.101358 0.975072 0.086 Uiso 1 1 calc R U . . .
N3 N 1.165(11) 0.331(11) 0.497(19) 0.081(15) Uani 1 1 d G U . . .
H3A H 1.282811 0.379738 0.500070 0.097 Uiso 1 1 calc R U . . .
C6 C 1.010(11) 0.391(11) 0.388(19) 0.073(14) Uani 1 1 d G U . . .
H6 H 1.012919 0.489729 0.304283 0.088 Uiso 1 1 calc R U . . .
N4 N 0.850(10) 0.278(12) 0.424(19) 0.067(13) Uani 1 1 d G U . . .
H4 H 0.733456 0.286098 0.372949 0.080 Uiso 1 1 calc R U . . .
C5 C 0.906(10) 0.149(11) 0.555(19) 0.071(15) Uani 1 1 d G U . . .
H5 H 0.824765 0.055604 0.604469 0.085 Uiso 1 1 calc R U . . .
C4 C 1.100(11) 0.182(11) 0.600(19) 0.080(16) Uani 1 1 d G U . . .
H4A H 1.176540 0.115518 0.685802 0.096 Uiso 1 1 calc R U . . .
C9 C 1.070(13) -0.317(13) 0.57(2) 0.102(18) Uani 1 1 d G U . . .
H9 H 1.144388 -0.398653 0.645746 0.122 Uiso 1 1 calc R U . . .
N5 N 1.143(12) -0.170(15) 0.49(3) 0.098(17) Uani 1 1 d G U . . .
H5A H 1.266848 -0.132671 0.500602 0.118 Uiso 1 1 calc R U . . .
C8 C 0.991(13) -0.089(13) 0.39(2) 0.095(17) Uani 1 1 d G U . . .
H8 H 0.999576 0.017120 0.320655 0.114 Uiso 1 1 calc R U . . .
C7 C 0.824(13) -0.187(13) 0.41(2) 0.089(17) Uani 1 1 d G U . . .
H7 H 0.695338 -0.161379 0.353059 0.106 Uiso 1 1 calc R U . . .
N6 N 0.873(12) -0.328(12) 0.52(2) 0.087(16) Uani 1 1 d G U . . .
H6A H 0.791470 -0.411414 0.551357 0.104 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br1 3.02(5) . ?
Pb1 Br2 3.04(4) . ?
Pb1 Br3 2.96(2) 1_655 ?
Pb1 Br3 3.01(2) . ?
Pb1 Br4 2.98(5) . ?
Pb1 Br5 2.97(5) . ?
C3 H3 0.9300 . ?
C3 N2 1.35(4) . ?
C3 C2 1.35(4) . ?
N2 H2 0.8600 . ?
N2 C1 1.36(4) . ?
C1 H1 0.9300 . ?
C1 N1 1.35(4) . ?
N1 H1A 0.8600 . ?
N1 C2 1.35(4) . ?
C2 H2A 0.9300 . ?
N3 H3A 0.8600 . ?
N3 C6 1.36(5) . ?
N3 C4 1.37(5) . ?
C6 H6 0.9300 . ?
C6 N4 1.36(5) . ?
N4 H4 0.8600 . ?
N4 C5 1.37(5) . ?
C5 H5 0.9300 . ?
C5 C4 1.35(5) . ?
C4 H4A 0.9300 . ?
C9 H9 0.9300 . ?
C9 N5 1.33(6) . ?
C9 N6 1.32(6) . ?
N5 H5A 0.8600 . ?
N5 C8 1.33(6) . ?
C8 H8 0.9300 . ?
C8 C7 1.33(6) . ?
C7 H7 0.9300 . ?
C7 N6 1.33(6) . ?
N6 H6A 0.8600 . ?

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 91.8(13) . . ?
Br1 Pb1 Br3 88.0(12) . 1_655 ?
Br1 Pb1 Br3 88.4(13) . . ?
Br1 Pb1 Br4 89.2(11) . . ?
Br1 Pb1 Br5 179.1(16) . . ?
Br2 Pb1 Br3 93.5(12) . 1_655 ?
Br2 Pb1 Br5 89.1(12) . . ?
Br3 Pb1 Br2 89.7(12) . . ?
Br3 Pb1 Br3 175(3) . 1_655 ?
Br3 Pb1 Br5 91.6(12) . . ?
Br4 Pb1 Br2 178.8(15) . . ?
Br4 Pb1 Br3 85.8(12) . 1_655 ?
Br4 Pb1 Br3 91.1(12) . . ?
Br4 Pb1 Br5 89.9(14) . . ?
Br5 Pb1 Br3 91.9(13) . 1_655 ?
Pb1 Br3 Pb1 175(3) . 1_455 ?
N2 C3 H3 126.2 . . ?
N2 C3 C2 107.6 . . ?
C2 C3 H3 126.2 . . ?
C3 N2 H2 125.9 . . ?
C3 N2 C1 108.2 . . ?
C1 N2 H2 125.9 . . ?
N2 C1 H1 125.9 . . ?
N1 C1 N2 108.2 . . ?
N1 C1 H1 125.9 . . ?
C1 N1 H1A 126.2 . . ?
C1 N1 C2 107.6 . . ?
C2 N1 H1A 126.2 . . ?
C3 C2 N1 108.51(6) . . ?
C3 C2 H2A 125.7 . . ?
N1 C2 H2A 125.7 . . ?
C6 N3 H3A 125.7 . . ?
C6 N3 C4 108.6 . . ?
C4 N3 H3A 125.7 . . ?
N3 C6 H6 126.4 . . ?
N4 C6 N3 107.3 . . ?
N4 C6 H6 126.4 . . ?
C6 N4 H4 125.7 . . ?
C6 N4 C5 108.6 . . ?
C5 N4 H4 125.7 . . ?
N4 C5 H5 126.1 . . ?
C4 C5 N4 107.8 . . ?
C4 C5 H5 126.1 . . ?
N3 C4 H4A 126.1 . . ?
C5 C4 N3 107.7 . . ?
C5 C4 H4A 126.1 . . ?
N5 C9 H9 126.1 . . ?
N6 C9 H9 126.2 . . ?
N6 C9 N5 107.7 . . ?
C9 N5 H5A 125.8 . . ?
C9 N5 C8 108.4 . . ?
C8 N5 H5A 125.8 . . ?
N5 C8 H8 126.2 . . ?
C7 C8 N5 107.7 . . ?
C7 C8 H8 126.2 . . ?
C8 C7 H7 126.0 . . ?
C8 C7 N6 108.1 . . ?
N6 C7 H7 126.0 . . ?
C9 N6 C7 108.1 . . ?
C9 N6 H6A 125.9 . . ?
C7 N6 H6A 125.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 N2 C1 N1 0.0 . . . . ?
N2 C3 C2 N1 0.0 . . . . ?
N2 C1 N1 C2 0.0 . . . . ?
C1 N1 C2 C3 0.0 . . . . ?
C2 C3 N2 C1 0.0 . . . . ?
N3 C6 N4 C5 0.0 . . . . ?
C6 N3 C4 C5 0.0 . . . . ?
C6 N4 C5 C4 0.0 . . . . ?
N4 C5 C4 N3 0.0 . . . . ?
C4 N3 C6 N4 0.0 . . . . ?
C9 N5 C8 C7 0.0 . . . . ?
N5 C9 N6 C7 0.0 . . . . ?
N5 C8 C7 N6 0.0 . . . . ?
C8 C7 N6 C9 0.0 . . . . ?
N6 C9 N5 C8 0.0 . . . . ?

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

data_im3pbbr5_155gpa
_database_code_depnum_ccdc_archive 'CCDC 2473981'
loop_
_audit_author_name
_audit_author_address
'Kinga Roszak'
;Adam Mickiewicz University Poznan
Poland
;
_audit_update_record             
;
2025-07-18 deposited with the CCDC.	2026-03-26 downloaded from the CCDC.
;
_audit_creation_date             2024-09-06
# start Validation Reply Form
_vrf_PLAT027_im3pbbr5_155gpa     
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      17.50 Degree
RESPONSE: A full set of data was collected, however 
the very high angle data was poor and was omitted.
Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the 
X-ray radiation to the measured sample.
;
_vrf_PLAT029_im3pbbr5_155gpa     
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.391 Why?  
RESPONSE: The data come from high-pressure studies and are 
limited by the DAC opening angle.
;
_vrf_PLAT090_im3pbbr5_155gpa     
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       3.49 Note  
RESPONSE:  The data/parameter ratio is affected by the access limits of the DAC.
;
_vrf_PLAT342_im3pbbr5_155gpa     
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.15667 Ang.  
RESPONSE: Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the X-ray 
radiation to the measured sample
;
_vrf_PLAT910_im3pbbr5_155gpa     
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         16 Note  
RESPONSE: These reflections were probably affected 
by unexpected deviations in their intensities for symmetry 
equivalent measurements and omitted during initial data reduction.
;
_vrf_PLAT911_im3pbbr5_155gpa     
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        848 Report
RESPONSE: These reflections were probably affected 
by unexpected deviations in their intensities for symmetry 
equivalent measurements and omitted during initial data reduction.
;
_vrf_PLAT915_im3pbbr5_155gpa     
;
PROBLEM: No Flack x Check Done: Low Friedel Pair Coverage         24 %     
RESPONSE: Because the Friedel Pair Coverage was low the absolute configuration was
assigned using the known absolute configuration of the molecules
;
_vrf_PLAT987_im3pbbr5_155gpa     
;
PROBLEM: The Flack x is >> 0 -  Do a BASF/TWIN Refinement     Please Check 
RESPONSE: As indicated by the Flack
parameter, the structures were refined as twins. 
All refinements converged to the racemic-twin compounds.
;
# end Validation Reply Form
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br5 Pb, 3(C3 H5 N2)'
_chemical_formula_sum            'C9 H15 Br5 N6 Pb'
_chemical_formula_weight         814.01
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   5.9377(5)
_cell_length_b                   9.139(2)
_cell_length_c                   9.150(3)
_cell_angle_alpha                66.16(3)
_cell_angle_beta                 84.388(17)
_cell_angle_gamma                87.214(15)
_cell_volume                     452.0(2)
_cell_formula_units_Z            1
_cell_measurement_pressure       1550000
_cell_measurement_reflns_used    1271
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.2100
_cell_measurement_theta_min      5.3270
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    20.383
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.00985
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
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    2.991
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             368
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_exptl_crystal_size_rad          0.400
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0672
_diffrn_reflns_av_unetI/netI     0.0842
_diffrn_reflns_Laue_measured_fraction_full 0.391
_diffrn_reflns_Laue_measured_fraction_max 0.308
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            2645
_diffrn_reflns_point_group_measured_fraction_full 0.391
_diffrn_reflns_point_group_measured_fraction_max 0.308
_diffrn_reflns_theta_full        17.500
_diffrn_reflns_theta_max         26.594
_diffrn_reflns_theta_min         5.343
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.2413
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.391
_diffrn_measured_fraction_theta_max 0.308
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  19.75   0.75   35.00   0.00 -30.00   0.00    --    73
  2  φ    140.00 200.00   0.75   35.00   0.00 -30.00   0.00    --    80
  3  φ    160.00 217.00   0.75   35.00   0.00  30.00   0.00    --    76
  4  φ    -20.00  34.75   0.75   35.00   0.00  30.00   0.00    --    73
  5  ω    -24.00  24.00   0.75   35.00    --   30.00  39.46 -12.90   64
  6  ω    -24.00  24.00   0.75   35.00    --   30.00  39.46 167.10   64
  7  ω    -50.00  10.00   0.75   35.00    --  -30.00  39.46 167.10   80
  8  ω    -50.00  10.00   0.75   35.00    --  -30.00  39.46 -12.90   80
  9  ω    -64.00  -8.50   0.75   35.00    --  -30.00  81.40 -28.90   74
 10  ω    -64.00  -8.50   0.75   35.00    --  -30.00  81.40 151.10   74
 11  ω    -19.00   8.00   0.75   35.00    --   30.00  81.40 151.10   36
 12  ω    -19.00   8.00   0.75   35.00    --   30.00  81.40 -28.90   36
 13  ω    -43.00 -21.25   0.75   35.00    --   30.00 134.60 -56.90   29
 14  ω    -43.00 -21.25   0.75   35.00    --   30.00 134.60 123.10   29
 15  ω    -90.00 -36.00   0.75   35.00    --  -30.00 134.60 123.10   72
 16  ω    -90.00 -36.00   0.75   35.00    --  -30.00 134.60 -56.90   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.391
_reflns_Friedel_fraction_max     0.308
_reflns_number_gt                740
_reflns_number_total             1030
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXD  (Sheldrick, 2008)'
_refine_diff_density_max         1.165
_refine_diff_density_min         -0.829
_refine_diff_density_rms         0.197
_refine_ls_abs_structure_details 
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack   0.5
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         1030
_refine_ls_number_restraints     264
_refine_ls_R_factor_all          0.1100
_refine_ls_R_factor_gt           0.0879
_refine_ls_restrained_S_all      0.949
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1655P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2244
_refine_ls_wR_factor_ref         0.2536
_refine_special_details          
;
 Refined as a 2-component perfect inversion twin.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Rigid bond restraints
 N5, C8, C7, N6, C9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N3, C6, N4, C5, C4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C2, N1, C1, N2, C3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Br2, Pb1, Br1, Br3, Br5, Br4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C9 \\sim N6 \\sim C7 \\sim C8 \\sim N5: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
C4 \\sim C5 \\sim N4 \\sim C6 \\sim N3: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
N1 \\sim C1 \\sim N2 \\sim C3 \\sim C2: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Br2 \\sim Br1 \\sim Pb1 \\sim Br3 \\sim Br5 \\sim Br4: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(C9) \\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim
Ueq, Uanis(N5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C4) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(N4) \\sim
Ueq, Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C2) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(N2) \\sim
Ueq, Uanis(C3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(Br2) \\sim Ueq, Uanis(Br1) \\sim Ueq, Uanis(Br4) \\sim Ueq, Uanis(Br3)
\\sim Ueq, Uanis(Pb1) \\sim Ueq, Uanis(Br5) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(N5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Br2) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
4.a :
 C3(N2,C1,N1,C2), N3(C6,N4,C5,C4), C9(N5,C8,C7,N6)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), N2(H2), C1(H1), N1(H1A), C2(H2A), N3(H3A), C6(H6), N4(H4), C5(H5),
 C4(H4A), C9(H9), N5(H5A), C8(H8), C7(H7), N6(H6A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 1.4914(11) 0.5020(14) -0.003(3) 0.077(4) Uani 1 1 d . U . . .
Br1 Br 1.480(3) 0.165(3) 0.256(6) 0.084(6) Uani 1 1 d . U . . .
Br2 Br 1.515(3) 0.378(3) -0.264(7) 0.087(6) Uani 1 1 d . U . . .
Br3 Br 0.989(4) 0.505(6) -0.013(10) 0.081(5) Uani 1 1 d . U . . .
Br4 Br 1.462(3) 0.626(3) 0.258(6) 0.079(7) Uani 1 1 d . U . . .
Br5 Br 1.503(3) 0.831(3) -0.243(6) 0.084(7) Uani 1 1 d . U . . .
C3 C 1.018(16) -0.127(10) 1.02(2) 0.070(15) Uani 1 1 d G U . . .
H3 H 1.035859 -0.236494 1.050269 0.084 Uiso 1 1 calc R U . . .
N2 N 1.169(10) -0.031(13) 1.03(2) 0.076(15) Uani 1 1 d G U . . .
H2 H 1.301857 -0.058462 1.064904 0.2(6) Uiso 1 1 calc R . . . .
C1 C 1.081(17) 0.114(11) 0.98(2) 0.076(15) Uani 1 1 d G U . . .
H1 H 1.151531 0.204311 0.979305 0.091 Uiso 1 1 calc R U . . .
N1 N 0.876(14) 0.108(12) 0.95(2) 0.075(15) Uani 1 1 d G U . . .
H1A H 0.783474 0.187433 0.910355 0.090 Uiso 1 1 calc R U . . .
C2 C 0.837(12) -0.040(13) 0.97(2) 0.073(15) Uani 1 1 d G U . . .
H2A H 0.704979 -0.077524 0.948900 0.088 Uiso 1 1 calc R U . . .
N3 N 1.184(19) 0.329(18) 0.50(3) 0.11(2) Uani 1 1 d G U . . .
H3A H 1.306174 0.376579 0.494127 0.137 Uiso 1 1 calc R U . . .
C6 C 1.03(2) 0.383(16) 0.38(3) 0.12(2) Uani 1 1 d G U . . .
H6 H 1.039249 0.476689 0.284652 0.139 Uiso 1 1 calc R U . . .
N4 N 0.855(14) 0.270(18) 0.43(3) 0.11(2) Uani 1 1 d G U . . .
H4 H 0.739066 0.274887 0.373849 0.135 Uiso 1 1 calc R U . . .
C5 C 0.902(19) 0.146(16) 0.57(2) 0.11(2) Uani 1 1 d G U . . .
H5 H 0.814468 0.056338 0.631168 0.132 Uiso 1 1 calc R U . . .
C4 C 1.105(17) 0.183(17) 0.62(2) 0.11(2) Uani 1 1 d G U . . .
H4A H 1.175698 0.121931 0.708000 0.132 Uiso 1 1 calc R U . . .
C9 C 1.069(15) -0.320(12) 0.55(2) 0.089(15) Uani 1 1 d G U . . .
H9 H 1.140870 -0.409248 0.618310 0.107 Uiso 1 1 calc R U . . .
N5 N 1.145(14) -0.168(12) 0.49(2) 0.084(15) Uani 1 1 d G U . . .
H5A H 1.267255 -0.136774 0.506250 0.101 Uiso 1 1 calc R U . . .
C8 C 0.993(14) -0.073(11) 0.38(2) 0.082(15) Uani 1 1 d G U . . .
H8 H 1.003658 0.037042 0.325930 0.099 Uiso 1 1 calc R U . . .
C7 C 0.824(13) -0.168(11) 0.38(2) 0.073(15) Uani 1 1 d G U . . .
H7 H 0.696746 -0.133577 0.327491 0.088 Uiso 1 1 calc R U . . .
N6 N 0.871(13) -0.320(11) 0.48(2) 0.076(14) Uani 1 1 d G U . . .
H6A H 0.790357 -0.402889 0.502816 0.092 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br1 3.03(4) . ?
Pb1 Br2 3.01(5) . ?
Pb1 Br3 2.95(2) 1_655 ?
Pb1 Br3 2.99(2) . ?
Pb1 Br4 3.02(4) . ?
Pb1 Br5 2.92(4) . ?
C3 H3 0.9300 . ?
C3 N2 1.32(5) . ?
C3 C2 1.32(5) . ?
N2 H2 0.8600 . ?
N2 C1 1.31(5) . ?
C1 H1 0.9300 . ?
C1 N1 1.31(5) . ?
N1 H1A 0.8600 . ?
N1 C2 1.31(5) . ?
C2 H2A 0.9300 . ?
N3 H3A 0.8600 . ?
N3 C6 1.41(9) . ?
N3 C4 1.41(9) . ?
C6 H6 0.9300 . ?
C6 N4 1.41(9) . ?
N4 H4 0.8900 . ?
N4 C5 1.41(9) . ?
C5 H5 0.9300 . ?
C5 C4 1.40(9) . ?
C4 H4A 0.9000 . ?
C9 H9 0.9300 . ?
C9 N5 1.35(7) . ?
C9 N6 1.36(7) . ?
N5 H5A 0.8400 . ?
N5 C8 1.36(7) . ?
C8 H8 0.9300 . ?
C8 C7 1.36(7) . ?
C7 H7 0.9100 . ?
C7 N6 1.35(7) . ?
N6 H6A 0.8600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br2 Pb1 Br1 91.7(13) . . ?
Br2 Pb1 Br4 179.4(7) . . ?
Br3 Pb1 Br1 90.8(13) 1_655 . ?
Br3 Pb1 Br1 91.3(12) . . ?
Br3 Pb1 Br2 91.5(11) 1_655 . ?
Br3 Pb1 Br2 86.0(12) . . ?
Br3 Pb1 Br3 177(3) 1_655 . ?
Br3 Pb1 Br4 93.4(11) . . ?
Br3 Pb1 Br4 89.1(12) 1_655 . ?
Br4 Pb1 Br1 88.3(11) . . ?
Br5 Pb1 Br1 177.8(15) . . ?
Br5 Pb1 Br2 90.5(12) . . ?
Br5 Pb1 Br3 89.0(12) . . ?
Br5 Pb1 Br3 89.0(12) . 1_655 ?
Br5 Pb1 Br4 89.4(13) . . ?
Pb1 Br3 Pb1 177(3) 1_455 . ?
N2 C3 H3 125.0 . . ?
N2 C3 C2 107.5 . . ?
C2 C3 H3 128.0 . . ?
C3 N2 H2 126.0 . . ?
C1 N2 C3 108.1 . . ?
C1 N2 H2 126.0 . . ?
N2 C1 H1 125.9 . . ?
N1 C1 N2 108.2 . . ?
N1 C1 H1 125.9 . . ?
C1 N1 H1A 126.0 . . ?
C1 N1 C2 107.9 . . ?
C2 N1 H1A 124.0 . . ?
C3 C2 H2A 125.9 . . ?
N1 C2 C3 108.2 . . ?
N1 C2 H2A 127.0 . . ?
C6 N3 H3A 124.0 . . ?
C6 N3 C4 108.12(7) . . ?
C4 N3 H3A 128.0 . . ?
N3 C6 H6 128.0 . . ?
N3 C6 N4 107.5 . . ?
N4 C6 H6 126.2 . . ?
C6 N4 H4 125.8 . . ?
C5 N4 C6 108.31(6) . . ?
C5 N4 H4 125.8 . . ?
N4 C5 H5 128.0 . . ?
C4 C5 N4 107.8 . . ?
C4 C5 H5 124.0 . . ?
N3 C4 H4A 125.9 . . ?
C5 C4 N3 107(14) . . ?
C5 C4 H4A 127.0 . . ?
N5 C9 H9 125.9 . . ?
N5 C9 N6 108.1 . . ?
N6 C9 H9 125.9 . . ?
C9 N5 H5A 127.0 . . ?
C9 N5 C8 107(10) . . ?
C8 N5 H5A 125.9 . . ?
N5 C8 H8 124.0 . . ?
C7 C8 N5 107.6 . . ?
C7 C8 H8 128.0 . . ?
C8 C7 H7 125.8 . . ?
N6 C7 C8 108.4 . . ?
N6 C7 H7 125.8 . . ?
C9 N6 H6A 124.0 . . ?
C7 N6 C9 109(11) . . ?
C7 N6 H6A 126.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 N2 C1 N1 4.0 . . . . ?
N2 C3 C2 N1 -0.4 . . . . ?
N2 C1 N1 C2 -4.0 . . . . ?
C1 N1 C2 C3 3.0 . . . . ?
C2 C3 N2 C1 -2(19) . . . . ?
N3 C6 N4 C5 -3.0 . . . . ?
C6 N3 C4 C5 0.3 . . . . ?
C6 N4 C5 C4 4.0 . . . . ?
N4 C5 C4 N3 -3.0 . . . . ?
C4 N3 C6 N4 1.0 . . . . ?
C9 N5 C8 C7 2(17) . . . . ?
N5 C9 N6 C7 -0.6 . . . . ?
N5 C8 C7 N6 -3(18) . . . . ?
C8 C7 N6 C9 3(18) . . . . ?
N6 C9 N5 C8 -1(16) . . . . ?

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

data_im3pbbr5_033gpa
_database_code_depnum_ccdc_archive 'CCDC 2473978'
loop_
_audit_author_name
_audit_author_address
'Kinga Roszak'
;Adam Mickiewicz University Poznan
Poland
;
_audit_update_record             
;
2025-07-18 deposited with the CCDC.	2026-03-26 downloaded from the CCDC.
;
_audit_creation_date             2024-08-27
# start Validation Reply Form
_vrf_PLAT027_im3pbbr5_033gpa     
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      17.50 Degree
RESPONSE: A full set of data was collected, however 
the very high angle data was poor and was omitted.
Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the 
X-ray radiation to the measured sample.
;
_vrf_PLAT029_im3pbbr5_033gpa     
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.327 Why?  
RESPONSE: The data come from high-pressure studies and are 
limited by the DAC opening angle.
;
_vrf_PLAT090_im3pbbr5_033gpa     
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       2.69 Note  
RESPONSE:  The data/parameter ratio is affected by the access limits of the DAC.
;
_vrf_PLAT342_im3pbbr5_033gpa     
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.10667 Ang.  
RESPONSE: Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the X-ray 
radiation to the measured sample
;
_vrf_PLAT910_im3pbbr5_033gpa     
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         16 Note  
RESPONSE: These reflections were probably affected 
by unexpected deviations in their intensities for symmetry 
equivalent measurements and omitted during initial data reduction.
;
_vrf_PLAT911_im3pbbr5_033gpa     
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        903 Report
RESPONSE: These reflections were probably affected 
by unexpected deviations in their intensities for symmetry 
equivalent measurements and omitted during initial data reduction.
;
_vrf_PLAT915_im3pbbr5_033gpa     
;
PROBLEM: No Flack x Check Done: Low Friedel Pair Coverage         21 %     
RESPONSE: Because the Friedel Pair Coverage was low the absolute configuration was
assigned using the known absolute configuration of the molecules
;
_vrf_PLAT987_im3pbbr5_033gpa     
;
PROBLEM: The Flack x is >> 0 -  Do a BASF/TWIN Refinement     Please Check 
RESPONSE: As indicated by the Flack
parameter, the structures were refined as twins. 
All refinements converged to the racemic-twin compounds.
;
# end Validation Reply Form
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br5 Pb, 3(C3 H5 N2)'
_chemical_formula_sum            'C9 H15 Br5 N6 Pb'
_chemical_formula_weight         813.97
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         C9H15Br5N6Pb
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   6.0296(6)
_cell_length_b                   9.308(2)
_cell_length_c                   9.546(4)
_cell_angle_alpha                66.89(3)
_cell_angle_beta                 85.91(2)
_cell_angle_gamma                88.101(18)
_cell_volume                     491.4(2)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    1129
_cell_measurement_pressure       330000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.2380
_cell_measurement_theta_min      5.1710
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    18.747
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.05789
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.750
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             368
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0544
_diffrn_reflns_av_unetI/netI     0.0683
_diffrn_reflns_Laue_measured_fraction_full 0.327
_diffrn_reflns_Laue_measured_fraction_max 0.231
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            2413
_diffrn_reflns_point_group_measured_fraction_full 0.327
_diffrn_reflns_point_group_measured_fraction_max 0.231
_diffrn_reflns_theta_full        17.500
_diffrn_reflns_theta_max         25.922
_diffrn_reflns_theta_min         5.196
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2413
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.327
_diffrn_measured_fraction_theta_max 0.231
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  19.75   0.75   35.00   0.00 -30.00   0.00    --    73
  2  φ    140.00 200.00   0.75   35.00   0.00 -30.00   0.00    --    80
  3  φ    160.00 217.00   0.75   35.00   0.00  30.00   0.00    --    76
  4  φ    -20.00  34.75   0.75   35.00   0.00  30.00   0.00    --    73
  5  ω    -24.00  24.00   0.75   35.00    --   30.00  39.46 -12.90   64
  6  ω    -24.00  24.00   0.75   35.00    --   30.00  39.46 167.10   64
  7  ω    -50.00  10.00   0.75   35.00    --  -30.00  39.46 167.10   80
  8  ω    -50.00  10.00   0.75   35.00    --  -30.00  39.46 -12.90   80
  9  ω    -64.00  -8.50   0.75   35.00    --  -30.00  81.40 -28.90   74
 10  ω    -64.00  -8.50   0.75   35.00    --  -30.00  81.40 151.10   74
 11  ω    -19.00   8.00   0.75   35.00    --   30.00  81.40 151.10   36
 12  ω    -19.00   8.00   0.75   35.00    --   30.00  81.40 -28.90   36
 13  ω    -43.00 -21.25   0.75   35.00    --   30.00 134.60 -56.90   29
 14  ω    -43.00 -21.25   0.75   35.00    --   30.00 134.60 123.10   29
 15  ω    -90.00 -36.00   0.75   35.00    --  -30.00 134.60 123.10   72
 16  ω    -90.00 -36.00   0.75   35.00    --  -30.00 134.60 -56.90   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0071827000
_diffrn_orient_matrix_UB_12      -0.0399664000
_diffrn_orient_matrix_UB_13      0.0805403000
_diffrn_orient_matrix_UB_21      -0.1168589000
_diffrn_orient_matrix_UB_22      0.0116368000
_diffrn_orient_matrix_UB_23      0.0012119000
_diffrn_orient_matrix_UB_31      -0.0142064000
_diffrn_orient_matrix_UB_32      -0.0716446000
_diffrn_orient_matrix_UB_33      -0.0080858000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.327
_reflns_Friedel_fraction_max     0.231
_reflns_number_gt                701
_reflns_number_total             850
_reflns_odcompleteness_completeness 22.42
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXD  (Sheldrick, 2008)'
_refine_diff_density_max         0.406
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details 
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack   0.5
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         850
_refine_ls_number_restraints     238
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0396
_refine_ls_restrained_S_all      0.935
_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)+(0.0444P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0790
_refine_ls_wR_factor_ref         0.0848
_refine_special_details          
;
 Refined as a 2-component perfect inversion twin.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 C9-C7
 2.2 with sigma of 0.02
3. Rigid bond restraints
 C2, C3, N2, C1, N1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C6, N4, N3, C5, C4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C8, C9, N5, C7, N6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C3 \\sim C1 \\sim N1 \\sim C2: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C6 \\sim N4 \\sim N3 \\sim C5 \\sim C4: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
N6 \\sim C9 \\sim N5 \\sim C8 \\sim C7: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C1) \\sim
Ueq, Uanis(N1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C6) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C5) \\sim
Ueq, Uanis(C4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C7) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(N6) \\sim
Ueq, Uanis(C8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(Br1) \\sim Ueq, Uanis(Br2) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(Br1) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(Br5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C3) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(Br3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Br4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Pb1) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(Br1) \\sim Ueq, Uanis(Br3) \\sim Ueq, Uanis(Br2) \\sim Ueq, Uanis(Br5)
\\sim Ueq, Uanis(Br4) \\sim Ueq: with sigma of 0.004 and sigma for terminal
atoms of 0.008
5.a :
 C3(N2,C1,N1,C2), N3(C6,N4,C5,C4), C9(N5,C8,C7,N6)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), N2(H2), C1(H1), N1(H1A), C2(H2A), N3(H3A), C6(H6), N4(H4), C5(H5),
 C4(H4A), C9(H9), N5(H5A), C8(H8), C7(H7), N6(H6A)
;
_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 1.4915(12) 0.4995(17) 0.003(3) 0.030(2) Uani 1 1 d . U . . .
Br1 Br 1.4800(19) 0.175(2) 0.244(4) 0.047(6) Uani 1 1 d . U . . .
Br2 Br 1.5105(17) 0.375(2) -0.249(4) 0.057(7) Uani 1 1 d . U . . .
Br3 Br 0.993(3) 0.496(5) 0.013(9) 0.042(3) Uani 1 1 d . U . . .
Br4 Br 1.4727(15) 0.6180(18) 0.254(4) 0.048(6) Uani 1 1 d . U . . .
Br5 Br 1.496(2) 0.832(2) -0.239(5) 0.055(6) Uani 1 1 d . U . . .
C3 C 0.961(9) -0.119(7) 1.001(13) 0.038(11) Uani 1 1 d G U . . .
H3 H 0.937225 -0.222429 1.014310 0.046 Uiso 1 1 calc R U . . .
N2 N 1.140(6) -0.065(7) 1.044(13) 0.054(12) Uani 1 1 d G U . . .
H2 H 1.251580 -0.119269 1.088031 0.065 Uiso 1 1 calc R U . . .
C1 C 1.110(7) 0.095(7) 1.003(12) 0.044(13) Uani 1 1 d G U . . .
H1 H 1.208405 0.161015 1.018907 0.053 Uiso 1 1 calc R U . . .
N1 N 0.913(8) 0.139(6) 0.935(12) 0.046(11) Uani 1 1 d G U . . .
H1A H 0.857384 0.231359 0.899524 0.055 Uiso 1 1 calc R U . . .
C2 C 0.821(6) 0.006(8) 0.934(12) 0.050(12) Uani 1 1 d G U . . .
H2A H 0.685662 0.001646 0.893965 0.060 Uiso 1 1 calc R U . . .
N3 N 1.164(6) 0.315(7) 0.523(13) 0.050(11) Uani 1 1 d G U . . .
H3A H 1.277869 0.367310 0.525374 0.060 Uiso 1 1 calc R U . . .
C6 C 1.007(7) 0.368(7) 0.420(13) 0.047(11) Uani 1 1 d G U . . .
H6 H 1.002072 0.464611 0.338792 0.056 Uiso 1 1 calc R U . . .
N4 N 0.859(7) 0.251(7) 0.457(12) 0.040(11) Uani 1 1 d G U . . .
H4 H 0.741843 0.253558 0.409263 0.048 Uiso 1 1 calc R U . . .
C5 C 0.924(7) 0.126(7) 0.584(13) 0.044(12) Uani 1 1 d G U . . .
H5 H 0.850442 0.031404 0.632446 0.052 Uiso 1 1 calc R U . . .
C4 C 1.113(7) 0.166(7) 0.625(13) 0.045(12) Uani 1 1 d G U . . .
H4A H 1.194266 0.104255 0.706919 0.054 Uiso 1 1 calc R U . . .
C9 C 1.072(9) -0.317(11) 0.603(16) 0.085(16) Uani 1 1 d DG U . . .
H9 H 1.140538 -0.385265 0.688573 0.102 Uiso 1 1 calc R U . . .
N5 N 1.144(8) -0.173(11) 0.507(18) 0.080(15) Uani 1 1 d G U . . .
H5A H 1.262412 -0.128875 0.516159 0.096 Uiso 1 1 calc R U . . .
C8 C 1.001(11) -0.109(9) 0.396(17) 0.086(17) Uani 1 1 d G U . . .
H8 H 1.012062 -0.011435 0.316026 0.104 Uiso 1 1 calc R U . . .
C7 C 0.840(9) -0.214(11) 0.422(16) 0.082(17) Uani 1 1 d DG U . . .
H7 H 0.719035 -0.201868 0.363787 0.099 Uiso 1 1 calc R U . . .
N6 N 0.884(9) -0.343(9) 0.551(16) 0.078(15) Uani 1 1 d G U . . .
H6A H 0.804641 -0.425694 0.590454 0.094 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 2.99(4) . ?
Pb1 Br2 3.04(4) . ?
Pb1 Br3 3.034(15) 1_655 ?
Pb1 Br3 2.999(15) . ?
Pb1 Br4 3.00(4) . ?
Pb1 Br5 3.05(4) . ?
C3 H3 0.9300 . ?
C3 N2 1.36(3) . ?
C3 C2 1.39(3) . ?
N2 H2 0.8600 . ?
N2 C1 1.39(3) . ?
C1 H1 0.9300 . ?
C1 N1 1.37(3) . ?
N1 H1A 0.8600 . ?
N1 C2 1.37(3) . ?
C2 H2A 0.9300 . ?
N3 H3A 0.8600 . ?
N3 C6 1.36(3) . ?
N3 C4 1.38(3) . ?
C6 H6 0.9300 . ?
C6 N4 1.35(3) . ?
N4 H4 0.8600 . ?
N4 C5 1.38(3) . ?
C5 H5 0.9300 . ?
C5 C4 1.34(3) . ?
C4 H4A 0.9300 . ?
C9 H9 0.9300 . ?
C9 N5 1.359(19) . ?
C9 N6 1.333(19) . ?
N5 H5A 0.8600 . ?
N5 C8 1.353(19) . ?
C8 H8 0.9300 . ?
C8 C7 1.337(19) . ?
C7 H7 0.9300 . ?
C7 N6 1.369(19) . ?
N6 H6A 0.8600 . ?

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 91.3(10) . . ?
Br3 Pb1 Br1 88.8(11) . . ?
Br3 Pb1 Br1 89.1(11) 1_655 . ?
Br3 Pb1 Br2 89.5(10) . . ?
Br3 Pb1 Br2 93.0(10) 1_655 . ?
Br3 Pb1 Br3 177(3) . 1_655 ?
Br4 Pb1 Br1 87.9(11) . . ?
Br4 Pb1 Br2 179.2(14) . . ?
Br4 Pb1 Br3 86.9(10) . 1_655 ?
Br4 Pb1 Br3 90.5(10) . . ?
Br4 Pb1 Br5 91.3(10) . . ?
Br5 Pb1 Br1 178.9(12) . . ?
Br5 Pb1 Br2 89.5(11) . . ?
Br5 Pb1 Br3 91.7(11) . 1_655 ?
Br5 Pb1 Br3 90.4(11) . . ?
Pb1 Br3 Pb1 177(3) . 1_455 ?
N2 C3 H3 126.3 . . ?
N2 C3 C2 107.5 . . ?
C2 C3 H3 126.3 . . ?
C3 N2 H2 126.1 . . ?
C3 N2 C1 107.9 . . ?
C1 N2 H2 126.1 . . ?
N2 C1 H1 125.6 . . ?
N1 C1 N2 108.8 . . ?
N1 C1 H1 125.6 . . ?
C1 N1 H1A 126.5 . . ?
C1 N1 C2 106.9 . . ?
C2 N1 H1A 126.5 . . ?
C3 C2 H2A 125.5 . . ?
N1 C2 C3 109.0 . . ?
N1 C2 H2A 125.5 . . ?
C6 N3 H3A 125.2 . . ?
C6 N3 C4 109.6 . . ?
C4 N3 H3A 125.2 . . ?
N3 C6 H6 126.9 . . ?
N4 C6 N3 106.2 . . ?
N4 C6 H6 126.9 . . ?
C6 N4 H4 125.4 . . ?
C6 N4 C5 109.3 . . ?
C5 N4 H4 125.4 . . ?
N4 C5 H5 126.1 . . ?
C4 C5 N4 107.7 . . ?
C4 C5 H5 126.1 . . ?
N3 C4 H4A 126.4 . . ?
C5 C4 N3 107.2 . . ?
C5 C4 H4A 126.4 . . ?
N5 C9 H9 126.5 . . ?
N6 C9 H9 126.5 . . ?
N6 C9 N5 107.0 . . ?
C9 N5 H5A 125.3 . . ?
C8 N5 C9 109.5 . . ?
C8 N5 H5A 125.3 . . ?
N5 C8 H8 126.7 . . ?
C7 C8 N5 106.7 . . ?
C7 C8 H8 126.7 . . ?
C8 C7 H7 125.7 . . ?
C8 C7 N6 108.7 . . ?
N6 C7 H7 125.7 . . ?
C9 N6 C7 108.2 . . ?
C9 N6 H6A 125.9 . . ?
C7 N6 H6A 125.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 N2 C1 N1 0.0 . . . . ?
N2 C3 C2 N1 0.0 . . . . ?
N2 C1 N1 C2 0.0 . . . . ?
C1 N1 C2 C3 0.0 . . . . ?
C2 C3 N2 C1 0.0 . . . . ?
N3 C6 N4 C5 0.0 . . . . ?
C6 N3 C4 C5 0.0 . . . . ?
C6 N4 C5 C4 0.0 . . . . ?
N4 C5 C4 N3 0.0 . . . . ?
C4 N3 C6 N4 0.0 . . . . ?
C9 N5 C8 C7 0.0 . . . . ?
N5 C9 N6 C7 0.0 . . . . ?
N5 C8 C7 N6 0.0 . . . . ?
C8 C7 N6 C9 0.0 . . . . ?
N6 C9 N5 C8 0.0 . . . . ?

_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 9.684
_oxdiff_exptl_absorpt_empirical_full_min 0.487
####################################################################### 
# 
# 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_im3pbbr5_060gpa
_database_code_depnum_ccdc_archive 'CCDC 2473979'
loop_
_audit_author_name
_audit_author_address
'Kinga Roszak'
;Adam Mickiewicz University Poznan
Poland
;
_audit_update_record             
;
2025-07-18 deposited with the CCDC.	2026-03-26 downloaded from the CCDC.
;
_audit_creation_date             2024-08-23
# start Validation Reply Form
_vrf_PLAT027_im3pbbr5_060gpa     
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      17.50 Degree
RESPONSE: A full set of data was collected, however 
the very high angle data was poor and was omitted.
Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the 
X-ray radiation to the measured sample.
;
_vrf_PLAT029_im3pbbr5_060gpa     
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.332 Why?  
RESPONSE: The data come from high-pressure studies and are 
limited by the DAC opening angle.
;
_vrf_PLAT090_im3pbbr5_060gpa     
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       2.66 Note  
RESPONSE:  The data/parameter ratio is affected by the access limits of the DAC.
;
_vrf_PLAT342_im3pbbr5_060gpa     
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............       0.11 Ang.  
RESPONSE: Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the X-ray 
radiation to the measured sample
;
_vrf_PLAT031_im3pbbr5_060gpa     
;
PROBLEM: Refined Extinction Parameter Within Range of ...      2.000 Sigma 
RESPONSE: Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the X-ray 
radiation to the measured sample
;
_vrf_PLAT910_im3pbbr5_060gpa     
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         16 Note  
RESPONSE: These reflections were probably affected 
by unexpected deviations in their intensities for symmetry 
equivalent measurements and omitted during initial data reduction.
;
_vrf_PLAT911_im3pbbr5_060gpa     
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        894 Report
RESPONSE: These reflections were probably affected 
by unexpected deviations in their intensities for symmetry 
equivalent measurements and omitted during initial data reduction.
;
_vrf_PLAT915_im3pbbr5_060gpa     
;
PROBLEM: No Flack x Check Done: Low Friedel Pair Coverage         21 %     
RESPONSE: Because the Friedel Pair Coverage was low the absolute configuration was
assigned using the known absolute configuration of the molecules
;
_vrf_PLAT987_im3pbbr5_060gpa     
;
PROBLEM: The Flack x is >> 0 -  Do a BASF/TWIN Refinement     Please Check 
RESPONSE: As indicated by the Flack
parameter, the structures were refined as twins. 
All refinements converged to the racemic-twin compounds.
;
# end Validation Reply Form
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br5 Pb, 3(C3 H5 N2)'
_chemical_formula_sum            'C9 H15 Br5 N6 Pb'
_chemical_formula_weight         813.97
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   6.0080(7)
_cell_length_b                   9.260(2)
_cell_length_c                   9.437(4)
_cell_angle_alpha                66.76(3)
_cell_angle_beta                 85.41(2)
_cell_angle_gamma                87.830(19)
_cell_volume                     480.9(3)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    1124
_cell_measurement_pressure       600000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.6900
_cell_measurement_theta_min      5.2200
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    19.160
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.00687
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.811
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             368
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0587
_diffrn_reflns_av_unetI/netI     0.0749
_diffrn_reflns_Laue_measured_fraction_full 0.332
_diffrn_reflns_Laue_measured_fraction_max 0.219
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            2469
_diffrn_reflns_point_group_measured_fraction_full 0.332
_diffrn_reflns_point_group_measured_fraction_max 0.219
_diffrn_reflns_theta_full        17.500
_diffrn_reflns_theta_max         26.633
_diffrn_reflns_theta_min         5.238
_diffrn_ambient_temperature      293(2)
_diffrn_ambient_environment      air
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_detector_area_resol_mean 16.2413
_diffrn_measured_fraction_theta_full 0.332
_diffrn_measured_fraction_theta_max 0.219
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0077084000
_diffrn_orient_matrix_UB_12      -0.0404622000
_diffrn_orient_matrix_UB_13      0.0815717000
_diffrn_orient_matrix_UB_21      -0.1173578000
_diffrn_orient_matrix_UB_22      0.0118197000
_diffrn_orient_matrix_UB_23      0.0015034000
_diffrn_orient_matrix_UB_31      -0.0140119000
_diffrn_orient_matrix_UB_32      -0.0719196000
_diffrn_orient_matrix_UB_33      -0.0082874000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  19.75   0.75   35.00   0.00 -30.00   0.00    --    73
  2  φ    140.00 200.00   0.75   35.00   0.00 -30.00   0.00    --    80
  3  φ    160.00 217.00   0.75   35.00   0.00  30.00   0.00    --    76
  4  φ    -20.00  34.75   0.75   35.00   0.00  30.00   0.00    --    73
  5  ω    -24.00  24.00   0.75   35.00    --   30.00  39.46 -12.90   64
  6  ω    -24.00  24.00   0.75   35.00    --   30.00  39.46 167.10   64
  7  ω    -50.00  10.00   0.75   35.00    --  -30.00  39.46 167.10   80
  8  ω    -50.00  10.00   0.75   35.00    --  -30.00  39.46 -12.90   80
  9  ω    -64.00  -8.50   0.75   35.00    --  -30.00  81.40 -28.90   74
 10  ω    -64.00  -8.50   0.75   35.00    --  -30.00  81.40 151.10   74
 11  ω    -19.00   8.00   0.75   35.00    --   30.00  81.40 151.10   36
 12  ω    -19.00   8.00   0.75   35.00    --   30.00  81.40 -28.90   36
 13  ω    -43.00 -21.25   0.75   35.00    --   30.00 134.60 -56.90   29
 14  ω    -43.00 -21.25   0.75   35.00    --   30.00 134.60 123.10   29
 15  ω    -90.00 -36.00   0.75   35.00    --  -30.00 134.60 123.10   72
 16  ω    -90.00 -36.00   0.75   35.00    --  -30.00 134.60 -56.90   72
;
_diffrn_measurement_method       'ω and φ scans'
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.332
_reflns_Friedel_fraction_max     0.219
_reflns_number_gt                707
_reflns_number_total             866
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXD  (Sheldrick, 2008)'
_refine_diff_density_max         0.427
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.110
_refine_ls_abs_structure_details 
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack   0.5
_refine_ls_extinction_coef       0.006(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         866
_refine_ls_number_restraints     237
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0441
_refine_ls_restrained_S_all      0.914
_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)+(0.0570P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0948
_refine_ls_wR_factor_ref         0.1030
_refine_special_details          
;
 Refined as a 2-component perfect inversion twin.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Rigid bond restraints
 N3, N4, C5, C6, C4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C2, C3, N2, C1, N1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N5, C9, N6, C8, C7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
N3 \\sim N4 \\sim C5 \\sim C6 \\sim C4: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
C2 \\sim C3 \\sim N2 \\sim C1 \\sim N1: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
N6 \\sim C9 \\sim N5 \\sim C8 \\sim C7: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Uanis(N3) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim
Ueq, Uanis(C4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C1) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C2) \\sim
Ueq, Uanis(N1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C9) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(C8) \\sim
Ueq, Uanis(C7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(Br1) \\sim Ueq, Uanis(Br2) \\sim Ueq, Uanis(Br5) \\sim Ueq, Uanis(Br4)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Br5) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(Br2) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(C7) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
4.a :
 C3(N2,C1,N1,C2), N3(C6,N4,C5,C4), C9(N5,C8,C7,N6)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), N2(H2), C1(H1), N1(H1A), C2(H2A), N3(H3A), C6(H6), N4(H4), C5(H5),
 C4(H4A), C9(H9), N5(H5A), C8(H8), C7(H7), N6(H6A)
;
_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 1.4888(13) 0.500(2) 0.003(4) 0.039(5) Uani 1 1 d . . . . .
Br1 Br 1.4779(19) 0.169(3) 0.250(5) 0.049(12) Uani 1 1 d . U . . .
Br2 Br 1.5144(17) 0.379(2) -0.256(5) 0.049(7) Uani 1 1 d . U . . .
Br3 Br 0.984(3) 0.497(6) 0.010(11) 0.045(14) Uani 1 1 d . . . . .
Br4 Br 1.4699(18) 0.623(2) 0.253(5) 0.049(12) Uani 1 1 d . U . . .
Br5 Br 1.496(2) 0.827(3) -0.234(5) 0.048(7) Uani 1 1 d . U . . .
C3 C 1.036(12) -0.136(7) 1.038(14) 0.042(13) Uani 1 1 d G U . . .
H3 H 1.067581 -0.240894 1.055061 0.051 Uiso 1 1 calc R U . . .
N2 N 1.168(6) -0.038(9) 1.066(14) 0.045(12) Uani 1 1 d G U . . .
H2 H 1.296802 -0.060839 1.103401 0.054 Uiso 1 1 calc R U . . .
C1 C 1.062(9) 0.104(7) 1.025(14) 0.031(12) Uani 1 1 d G U . . .
H1 H 1.116292 0.192775 1.032804 0.037 Uiso 1 1 calc R U . . .
N1 N 0.864(7) 0.093(8) 0.972(14) 0.041(12) Uani 1 1 d G U . . .
H1A H 0.766302 0.166940 0.938663 0.049 Uiso 1 1 calc R U . . .
C2 C 0.848(9) -0.055(8) 0.979(15) 0.044(13) Uani 1 1 d G U . . .
H2A H 0.728614 -0.095209 0.949733 0.052 Uiso 1 1 calc R U . . .
N3 N 1.163(9) 0.322(10) 0.502(16) 0.063(15) Uani 1 1 d G U . . .
H3A H 1.281196 0.365638 0.510647 0.076 Uiso 1 1 calc R U . . .
C6 C 1.022(9) 0.385(9) 0.389(16) 0.050(14) Uani 1 1 d G U . . .
H6 H 1.033979 0.483184 0.307991 0.060 Uiso 1 1 calc R U . . .
N4 N 0.861(7) 0.280(9) 0.417(16) 0.037(12) Uani 1 1 d G U . . .
H4 H 0.748943 0.291521 0.361675 0.045 Uiso 1 1 calc R U . . .
C5 C 0.902(8) 0.151(9) 0.547(16) 0.044(14) Uani 1 1 d G U . . .
H5 H 0.814730 0.061561 0.590565 0.053 Uiso 1 1 calc R U . . .
C4 C 1.088(9) 0.177(9) 0.599(16) 0.061(15) Uani 1 1 d G U . . .
H4A H 1.155931 0.109047 0.686128 0.073 Uiso 1 1 calc R U . . .
C9 C 1.047(10) -0.333(11) 0.585(17) 0.064(14) Uani 1 1 d G U . . .
H9 H 1.106327 -0.419010 0.663775 0.076 Uiso 1 1 calc R U . . .
N5 N 1.138(9) -0.194(11) 0.514(19) 0.061(14) Uani 1 1 d G U . . .
H5A H 1.263549 -0.166327 0.532715 0.073 Uiso 1 1 calc R U . . .
C8 C 1.006(10) -0.104(9) 0.410(18) 0.053(14) Uani 1 1 d G U . . .
H8 H 1.030727 0.000751 0.343812 0.064 Uiso 1 1 calc R U . . .
C7 C 0.833(9) -0.187(9) 0.417(16) 0.050(13) Uani 1 1 d G U . . .
H7 H 0.712384 -0.152890 0.355544 0.060 Uiso 1 1 calc R U . . .
N6 N 0.859(9) -0.329(9) 0.525(17) 0.049(12) Uani 1 1 d G U . . .
H6A H 0.766536 -0.405718 0.551060 0.059 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br1 3.03(4) . ?
Pb1 Br2 3.06(4) . ?
Pb1 Br3 2.979(19) 1_655 ?
Pb1 Br3 3.030(18) . ?
Pb1 Br4 2.99(4) . ?
Pb1 Br5 2.97(4) . ?
C3 H3 0.9300 . ?
C3 N2 1.34(3) . ?
C3 C2 1.36(3) . ?
N2 H2 0.8600 . ?
N2 C1 1.36(3) . ?
C1 H1 0.9300 . ?
C1 N1 1.35(3) . ?
N1 H1A 0.8600 . ?
N1 C2 1.35(3) . ?
C2 H2A 0.9300 . ?
N3 H3A 0.8600 . ?
N3 C6 1.34(4) . ?
N3 C4 1.36(4) . ?
C6 H6 0.9300 . ?
C6 N4 1.34(4) . ?
N4 H4 0.8600 . ?
N4 C5 1.36(4) . ?
C5 H5 0.9300 . ?
C5 C4 1.33(4) . ?
C4 H4A 0.9300 . ?
C9 H9 0.9300 . ?
C9 N5 1.31(4) . ?
C9 N6 1.30(4) . ?
N5 H5A 0.8600 . ?
N5 C8 1.31(4) . ?
C8 H8 0.9300 . ?
C8 C7 1.30(4) . ?
C7 H7 0.9300 . ?
C7 N6 1.32(4) . ?
N6 H6A 0.8600 . ?

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 92.1(11) . . ?
Br1 Pb1 Br3 89.3(13) . . ?
Br3 Pb1 Br1 89.1(13) 1_655 . ?
Br3 Pb1 Br2 92.5(12) 1_655 . ?
Br3 Pb1 Br2 89.3(12) . . ?
Br3 Pb1 Br3 178(3) 1_655 . ?
Br3 Pb1 Br4 86.8(12) 1_655 . ?
Br4 Pb1 Br1 88.8(12) . . ?
Br4 Pb1 Br2 178.9(14) . . ?
Br4 Pb1 Br3 91.4(12) . . ?
Br5 Pb1 Br1 178.7(15) . . ?
Br5 Pb1 Br2 89.2(12) . . ?
Br5 Pb1 Br3 90.4(13) . . ?
Br5 Pb1 Br3 91.1(13) . 1_655 ?
Br5 Pb1 Br4 89.9(11) . . ?
Pb1 Br3 Pb1 178(3) 1_455 . ?
N2 C3 H3 126.2 . . ?
N2 C3 C2 107.6 . . ?
C2 C3 H3 126.2 . . ?
C3 N2 H2 126.0 . . ?
C3 N2 C1 107.9 . . ?
C1 N2 H2 126.0 . . ?
N2 C1 H1 125.7 . . ?
N1 C1 N2 108.5 . . ?
N1 C1 H1 125.7 . . ?
C1 N1 H1A 126.4 . . ?
C1 N1 C2 107.2 . . ?
C2 N1 H1A 126.4 . . ?
C3 C2 H2A 125.6 . . ?
N1 C2 C3 108.7 . . ?
N1 C2 H2A 125.6 . . ?
C6 N3 H3A 125.4 . . ?
C6 N3 C4 109.3 . . ?
C4 N3 H3A 125.4 . . ?
N3 C6 H6 126.7 . . ?
N4 C6 N3 106.6 . . ?
N4 C6 H6 126.7 . . ?
C6 N4 H4 125.5 . . ?
C6 N4 C5 108.9 . . ?
C5 N4 H4 125.5 . . ?
N4 C5 H5 126.1 . . ?
C4 C5 N4 107.8 . . ?
C4 C5 H5 126.1 . . ?
N3 C4 H4A 126.3 . . ?
C5 C4 N3 107.3 . . ?
C5 C4 H4A 126.3 . . ?
N5 C9 H9 126.4 . . ?
N6 C9 H9 126.4 . . ?
N6 C9 N5 107.2 . . ?
C9 N5 H5A 125.5 . . ?
C8 N5 C9 109.1 . . ?
C8 N5 H5A 125.5 . . ?
N5 C8 H8 126.5 . . ?
C7 C8 N5 107.1 . . ?
C7 C8 H8 126.5 . . ?
C8 C7 H7 125.8 . . ?
C8 C7 N6 108.4 . . ?
N6 C7 H7 125.8 . . ?
C9 N6 C7 108.2 . . ?
C9 N6 H6A 125.9 . . ?
C7 N6 H6A 125.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 N2 C1 N1 0.0 . . . . ?
N2 C3 C2 N1 0.0 . . . . ?
N2 C1 N1 C2 0.0 . . . . ?
C1 N1 C2 C3 0.0 . . . . ?
C2 C3 N2 C1 0.0 . . . . ?
N3 C6 N4 C5 0.1 . . . . ?
C6 N3 C4 C5 0.0 . . . . ?
C6 N4 C5 C4 0.0 . . . . ?
N4 C5 C4 N3 0.0 . . . . ?
C4 N3 C6 N4 -0.1 . . . . ?
C9 N5 C8 C7 0.0 . . . . ?
N5 C9 N6 C7 0.0 . . . . ?
N5 C8 C7 N6 0.0 . . . . ?
C8 C7 N6 C9 0.0 . . . . ?
N6 C9 N5 C8 0.0 . . . . ?

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

data_im2pbbr4_1_12gpa
_database_code_depnum_ccdc_archive 'CCDC 2473970'
loop_
_audit_author_name
_audit_author_address
'Kinga Roszak'
;Adam Mickiewicz University Poznan
Poland
;
_audit_update_record             
;
2025-07-18 deposited with the CCDC.	2026-03-26 downloaded from the CCDC.
;
_audit_creation_date             2023-04-11
# start Validation Reply Form
_vrf_PLAT027_im2pbbr4_1_12gpa    
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      17.50 Degree
RESPONSE: A full set of data was collected, however 
the very high angle data was poor and was omitted.
Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the 
X-ray radiation to the measured sample.
;
_vrf_PLAT029_im2pbbr4_1_12gpa    
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.318 Why?  
RESPONSE: The data come from high-pressure studies and are 
limited by the DAC opening angle.
;
_vrf_PLAT088_im2pbbr4_1_12gpa    
;
PROBLEM: Poor Data / Parameter Ratio ....................       5.54 Note  
RESPONSE: The data/parameter ratio is affected by the access limits of the DAC.
;
_vrf_PLAT342_im2pbbr4_1_12gpa    
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............      0.055 Ang.  
RESPONSE: Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the X-ray 
radiation to the measured sample; poor quality of measurement
;
_vrf_PLAT911_im2pbbr4_1_12gpa    
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        649 Report
RESPONSE: These reflections were probably affected 
by unexpected deviations in their intensities for symmetry 
equivalent measurements and omitted during initial data reduction.
;
# end Validation Reply Form
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br4 Pb, 2(C3 H5 N2)'
_chemical_formula_sum            'C6 H10 Br4 N4 Pb'
_chemical_formula_weight         665.01
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   5.9525(5)
_cell_length_b                   9.1849(15)
_cell_length_c                   13.074(5)
_cell_angle_alpha                73.89(2)
_cell_angle_beta                 85.092(17)
_cell_angle_gamma                87.626(10)
_cell_volume                     684.1(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1223
_cell_measurement_temperature    293(2)
_cell_measurement_pressure       1120000
_cell_measurement_theta_max      23.3450
_cell_measurement_theta_min      3.4020
_shelx_estimated_absorpt_T_max   0.327
_shelx_estimated_absorpt_T_min   0.073
_exptl_absorpt_coefficient_mu    23.989
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7331
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.89a (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_density_diffrn    3.228
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1305
_diffrn_reflns_av_unetI/netI     0.0915
_diffrn_reflns_Laue_measured_fraction_full 0.318
_diffrn_reflns_Laue_measured_fraction_max 0.189
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            6736
_diffrn_reflns_point_group_measured_fraction_full 0.318
_diffrn_reflns_point_group_measured_fraction_max 0.189
_diffrn_reflns_theta_full        17.500
_diffrn_reflns_theta_max         28.649
_diffrn_reflns_theta_min         2.308
_diffrn_ambient_temperature      293(2)
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_detector_area_resol_mean 16.1544
_diffrn_measured_fraction_theta_full 0.318
_diffrn_measured_fraction_theta_max 0.189
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0027121000
_diffrn_orient_matrix_UB_12      0.0148728000
_diffrn_orient_matrix_UB_13      0.0505136000
_diffrn_orient_matrix_UB_21      0.0303709000
_diffrn_orient_matrix_UB_22      -0.0767000000
_diffrn_orient_matrix_UB_23      0.0237653000
_diffrn_orient_matrix_UB_31      0.1156678000
_diffrn_orient_matrix_UB_32      0.0189520000
_diffrn_orient_matrix_UB_33      -0.0095746000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      9.00  47.40   0.80   20.00    --   17.47 -77.00-150.00   48
  2  ω     19.00  79.00   0.80   20.00    --   17.47-134.00  56.00   75
  3  ω    -31.00  47.40   0.80   20.00    --   17.47 -26.00   7.00   98
  4  ω    -27.00  26.60   0.80   20.00    --   17.47  19.00-180.00   67
  5  ω     29.00  57.00   0.80   20.00    --   17.47 -99.00  60.00   35
  6  ω     -8.00  26.40   0.80   20.00    --   17.47  39.00 -12.00   43
  7  ω     -4.00  28.00   0.80   20.00    --   17.47  57.00 150.00   40
  8  ω    -45.00  15.00   0.80   20.00    --  -18.72  37.00-180.00   75
  9  ω    -39.00  38.60   0.80   20.00    --  -18.72   0.00   0.00   97
 10  ω    -81.00 -17.00   0.80   20.00    --  -18.72 134.00 123.00   80
 11  ω    -14.00  10.00   0.80   20.00    --  -18.72 -77.00-150.00   30
 12  ω     17.00  42.60   0.80   20.00    --  -18.72-134.00  56.00   32
 13  ω    -31.00  13.00   0.80   20.00    --  -18.72 -26.00-172.00   55
 14  ω    -35.00 -15.00   0.80   20.00    --  -18.72  37.00 -30.00   25
 15  ω     17.00  42.60   0.80   20.00    --  -18.72-134.00-123.00   32
 16  ω     29.00  57.00   0.80   20.00    --   17.47 -99.00  30.00   35
 17  ω     30.00  57.20   0.80   20.00    --   17.47 -99.00   0.00   34
 18  ω     30.00  57.20   0.80   20.00    --   17.47 -99.00-180.00   34
 19  ω    -45.00 -17.00   0.80   20.00    --   17.47 134.00 -56.00   35
 20  ω     54.00  94.00   0.80   20.00    --   17.47-178.00 -90.00   50
 21  ω     29.00  57.00   0.80   20.00    --   17.47 -99.00-120.00   35
 22  ω     -4.00  44.00   0.80   20.00    --   17.47  57.00 -60.00   60
 23  ω    -15.00  30.60   0.80   20.00    --   17.47  26.00  -7.00   57
 24  ω    -31.00  13.00   0.80   20.00    --  -18.72 -26.00   7.00   55
 25  ω    -43.00  17.00   0.80   20.00    --  -18.72  67.00 -23.00   75
 26  ω    -52.00  -4.00   0.80   20.00    --  -18.72  19.00-150.00   60
 27  ω    -28.00   2.40   0.80   20.00    --  -18.72 -57.00  30.00   38
 28  ω    -21.20  38.00   0.80   20.00    --   17.47 -53.00-162.00   74
 29  ω     -4.00  38.40   0.80   20.00    --   17.47 -57.00-180.00   53
 30  ω    -27.00  51.40   0.80   20.00    --   17.47 -19.00-180.00   98
 31  ω    -51.00  10.60   0.80   20.00    --  -18.72  81.00 -29.00   77
;
_diffrn_measurement_method       'ω scans'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                440
_reflns_number_total             665
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.922
_refine_diff_density_min         -0.713
_refine_diff_density_rms         0.176
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         665
_refine_ls_number_restraints     141
_refine_ls_R_factor_all          0.1067
_refine_ls_R_factor_gt           0.0595
_refine_ls_restrained_S_all      0.952
_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)+(0.0881P)²+4.6095P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1367
_refine_ls_wR_factor_ref         0.1608
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 N3-C4
 1.308 with sigma of 0.02
3. Rigid bond restraints
 C2, N2, C3, C1, N1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C6, C4, N3, C5, N4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
N1 \\sim C1 \\sim C3 \\sim N2 \\sim C2: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
C5 \\sim N3 \\sim C4 \\sim C6 \\sim N4: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Uanis(N3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C5) \\sim
Ueq, Uanis(N4) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of
0.008
Uanis(N1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C3) \\sim
Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of
0.008
5.a :
 C2(N2,C3,C1,N1), C4(N3,C5,N4,C6)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), N2(H2A), C3(H3), C1(H1), N1(H1A), C4(H4), N3(H3A), C5(H5), N4(H4A),
 C6(H6)
;
_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 0.51188(17) 0.57508(15) 0.3273(3) 0.032(5) Uani 1 1 d . . . . .
Br1 Br 0.4960(6) 0.7281(5) 0.5003(10) 0.053(12) Uani 1 1 d . . . . .
Br2 Br 0.0120(4) 0.5720(4) 0.3346(9) 0.037(12) Uani 1 1 d . . . . .
Br3 Br 0.5103(6) 0.8699(4) 0.1714(10) 0.039(12) Uani 1 1 d . . . . .
Br4 Br 0.5311(6) 0.4087(5) 0.1636(11) 0.062(13) Uani 1 1 d . . . . .
C2 C 1.036(6) 0.664(3) 0.058(6) 0.086(9) Uani 1 1 d G U . . .
H2 H 1.078969 0.580197 0.111276 0.103 Uiso 1 1 calc R U . . .
N2 N 1.142(5) 0.793(4) 0.025(7) 0.088(9) Uani 1 1 d G U . . .
H2A H 1.262296 0.815081 0.049399 0.105 Uiso 1 1 calc R U . . .
C3 C 1.029(6) 0.881(4) -0.050(7) 0.087(9) Uani 1 1 d G U . . .
H3 H 1.066256 0.979932 -0.087869 0.104 Uiso 1 1 calc R U . . .
C1 C 0.853(5) 0.807(4) -0.065(6) 0.081(9) Uani 1 1 d G U . . .
H1 H 0.746614 0.844535 -0.113977 0.097 Uiso 1 1 calc R U . . .
N1 N 0.858(5) 0.673(4) 0.002(6) 0.083(9) Uani 1 1 d G U . . .
H1A H 0.762002 0.602735 0.009195 0.100 Uiso 1 1 calc R U . . .
C4 C 0.065(6) 0.177(3) 0.352(6) 0.070(8) Uani 1 1 d DG U . . .
H4 H 0.118308 0.270416 0.351560 0.084 Uiso 1 1 calc R U . . .
N3 N -0.113(5) 0.153(3) 0.309(6) 0.073(8) Uani 1 1 d DG U . . .
H3A H -0.204197 0.221475 0.275297 0.088 Uiso 1 1 calc R U . . .
C5 C -0.130(5) 0.005(3) 0.326(6) 0.072(8) Uani 1 1 d G U . . .
H5 H -0.243817 -0.042604 0.303579 0.087 Uiso 1 1 calc R U . . .
N4 N 0.038(5) -0.063(3) 0.379(6) 0.073(8) Uani 1 1 d G U . . .
H4A H 0.063607 -0.158627 0.399996 0.088 Uiso 1 1 calc R U . . .
C6 C 0.158(5) 0.043(3) 0.395(6) 0.068(8) Uani 1 1 d G U . . .
H6 H 0.289186 0.027463 0.431178 0.082 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 2.969(15) . ?
Pb1 Br1 3.058(6) 2_666 ?
Pb1 Br2 2.970(3) . ?
Pb1 Br2 2.986(3) 1_655 ?
Pb1 Br3 2.902(5) . ?
Pb1 Br4 2.947(15) . ?
C2 H2 0.9300 . ?
C2 N2 1.31(2) . ?
C2 N1 1.32(2) . ?
N2 H2A 0.8600 . ?
N2 C3 1.31(2) . ?
C3 H3 0.9300 . ?
C3 C1 1.32(2) . ?
C1 H1 0.9300 . ?
C1 N1 1.30(2) . ?
N1 H1A 0.8600 . ?
C4 H4 0.9300 . ?
C4 N3 1.294(16) . ?
C4 C6 1.319(16) . ?
N3 H3A 0.8600 . ?
N3 C5 1.320(16) . ?
C5 H5 0.9300 . ?
C5 N4 1.304(16) . ?
N4 H4A 0.8600 . ?
N4 C6 1.304(16) . ?
C6 H6 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br1 Pb1 Br1 88.1(2) . 2_666 ?
Br1 Pb1 Br2 91.8(3) . . ?
Br1 Pb1 Br2 85.7(2) . 1_655 ?
Br2 Pb1 Br1 88.16(13) 1_655 2_666 ?
Br2 Pb1 Br1 89.30(13) . 2_666 ?
Br2 Pb1 Br2 176.5(5) . 1_655 ?
Br3 Pb1 Br1 177.2(3) . 2_666 ?
Br3 Pb1 Br1 89.3(3) . . ?
Br3 Pb1 Br2 89.80(12) . . ?
Br3 Pb1 Br2 92.63(13) . 1_655 ?
Br3 Pb1 Br4 93.5(3) . . ?
Br4 Pb1 Br1 177.14(19) . . ?
Br4 Pb1 Br1 89.1(3) . 2_666 ?
Br4 Pb1 Br2 88.6(2) . . ?
Br4 Pb1 Br2 93.8(2) . 1_655 ?
Pb1 Br1 Pb1 91.9(2) . 2_666 ?
Pb1 Br2 Pb1 176.5(5) . 1_455 ?
N2 C2 H2 125.5 . . ?
N2 C2 N1 109.0 . . ?
N1 C2 H2 125.5 . . ?
C2 N2 H2A 126.6 . . ?
C2 N2 C3 106.7 . . ?
C3 N2 H2A 126.6 . . ?
N2 C3 H3 125.5 . . ?
N2 C3 C1 109.1 . . ?
C1 C3 H3 125.5 . . ?
C3 C1 H1 126.3 . . ?
N1 C1 C3 107.5 . . ?
N1 C1 H1 126.3 . . ?
C2 N1 H1A 126.2 . . ?
C1 N1 C2 107.7 . . ?
C1 N1 H1A 126.2 . . ?
N3 C4 H4 126.2 . . ?
N3 C4 C6 107.6 . . ?
C6 C4 H4 126.2 . . ?
C4 N3 H3A 126.2 . . ?
C4 N3 C5 107.7 . . ?
C5 N3 H3A 126.2 . . ?
N3 C5 H5 125.5 . . ?
N4 C5 N3 108.9 . . ?
N4 C5 H5 125.5 . . ?
C5 N4 H4A 126.6 . . ?
C5 N4 C6 106.8 . . ?
C6 N4 H4A 126.6 . . ?
C4 C6 H6 125.5 . . ?
N4 C6 C4 109.0 . . ?
N4 C6 H6 125.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 N2 C3 C1 0.0 . . . . ?
N2 C2 N1 C1 0.1 . . . . ?
N2 C3 C1 N1 0.1 . . . . ?
C3 C1 N1 C2 -0.1 . . . . ?
N1 C2 N2 C3 1(8) . . . . ?
C4 N3 C5 N4 0.0 . . . . ?
N3 C4 C6 N4 0.0 . . . . ?
N3 C5 N4 C6 0.0 . . . . ?
C5 N4 C6 C4 0.0 . . . . ?
C6 C4 N3 C5 0.0 . . . . ?

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

data_im2pbbr4_5_26gpa
_database_code_depnum_ccdc_archive 'CCDC 2473977'
loop_
_audit_author_name
_audit_author_address
'Kinga Roszak'
;Adam Mickiewicz University Poznan
Poland
;
_audit_update_record             
;
2025-07-18 deposited with the CCDC.	2026-03-26 downloaded from the CCDC.
;
_audit_creation_date             2023-07-21
# start Validation Reply Form
_vrf_RINTA01_im2pbbr4_5_26gpa    
;
PROBLEM: The value of Rint is greater than 0.25
RESPONSE: High factor is a result from the weak diffraction. Due to the specificity 
of the applied measuring technique and use of a diamond-anvil cell 
limiting the access of the X-ray radiation to the measured sample.
;
_vrf_PLAT020_im2pbbr4_5_26gpa    
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.255 Report
RESPONSE: High factor is a result from the weak diffraction. Due to the specificity 
of the applied measuring technique and use of a diamond-anvil cell 
limiting the access of the X-ray radiation to the measured sample.
;
_vrf_PLAT027_im2pbbr4_5_26gpa    
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      17.50 Degree
RESPONSE: A full set of data was collected, however 
the very high angle data was poor and was omitted.
Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the 
X-ray radiation to the measured sample.
;
_vrf_PLAT029_im2pbbr4_5_26gpa    
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.293 Why?  
RESPONSE: The data come from high-pressure studies and are 
limited by the DAC opening angle.
;
_vrf_PLAT088_im2pbbr4_5_26gpa    
;
PROBLEM: Poor Data / Parameter Ratio ....................       4.47 Note  
RESPONSE: The data/parameter ratio is affected by the access limits of the DAC.
;
_vrf_PLAT411_im2pbbr4_5_26gpa    
;
PROBLEM: Short Inter H...H Contact  H3       ..H3       .       1.64 Ang.  
RESPONSE: It is very difficult to locate hydrogen atoms 
accurately using X-ray data because these atoms have low 
scattering power. In addition, we have bad quality measurement 
and low resolution data.
;
_vrf_PLAT342_im2pbbr4_5_26gpa    
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............      0.075 Ang.  
RESPONSE: Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the X-ray 
radiation to the measured sample; poor quality of measurement
;
_vrf_PLAT911_im2pbbr4_5_26gpa    
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        474 Report
RESPONSE: These reflections were probably affected 
by unexpected deviations in their intensities for symmetry 
equivalent measurements and omitted during initial data reduction.
;
# end Validation Reply Form
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br4 Pb, 2(C3 H5 N2)'
_chemical_formula_sum            'C6 H10 Br4 N4 Pb'
_chemical_formula_weight         665.01
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   5.732(4)
_cell_length_b                   9.062(8)
_cell_length_c                   12.225(19)
_cell_angle_alpha                71.26(13)
_cell_angle_beta                 81.11(13)
_cell_angle_gamma                84.70(7)
_cell_volume                     593.5(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    444
_cell_measurement_pressure       5260000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.3330
_cell_measurement_theta_min      3.5020
_shelx_estimated_absorpt_T_max   0.288
_shelx_estimated_absorpt_T_min   0.061
_exptl_absorpt_coefficient_mu    27.653
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.7115
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.89a (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_density_diffrn    3.721
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.2549
_diffrn_reflns_av_unetI/netI     0.1766
_diffrn_reflns_Laue_measured_fraction_full 0.293
_diffrn_reflns_Laue_measured_fraction_max 0.188
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            5514
_diffrn_reflns_point_group_measured_fraction_full 0.293
_diffrn_reflns_point_group_measured_fraction_max 0.188
_diffrn_reflns_theta_full        17.500
_diffrn_reflns_theta_max         27.955
_diffrn_reflns_theta_min         2.376
_diffrn_ambient_temperature      293(2)
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_detector_area_resol_mean 16.1544
_diffrn_measured_fraction_theta_full 0.293
_diffrn_measured_fraction_theta_max 0.188
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0145959000
_diffrn_orient_matrix_UB_12      0.0038305000
_diffrn_orient_matrix_UB_13      0.0572543000
_diffrn_orient_matrix_UB_21      0.0323374000
_diffrn_orient_matrix_UB_22      -0.0805042000
_diffrn_orient_matrix_UB_23      0.0207489000
_diffrn_orient_matrix_UB_31      0.1195868000
_diffrn_orient_matrix_UB_32      0.0183013000
_diffrn_orient_matrix_UB_33      -0.0070938000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -3.00  19.40   0.70   14.00    --   17.94  57.00 -30.00   32
  2  ω    -31.00   0.50   0.70   14.00    --   17.94   0.00-150.00   45
  3  ω     -8.00  43.10   0.70   14.00    --   17.94 -37.00-180.00   73
  4  ω    -34.00  26.20   0.70   14.00    --   17.94  13.00  -3.00   86
  5  ω    -20.00   2.40   0.70   14.00    --  -18.72 -57.00-150.00   32
  6  ω    -23.00  13.40   0.70   14.00    --  -18.72 -26.00-172.00   52
  7  ω    -81.00 -25.00   0.70   14.00    --  -18.72 134.00 -56.00   80
  8  ω    -23.00  13.40   0.70   14.00    --  -18.72 -26.00   7.00   52
  9  ω    -44.00  18.30   0.70   14.00    --  -18.72  39.00 167.00   89
 10  ω    -81.00 -25.00   0.70   14.00    --  -18.72 134.00 123.00   80
 11  ω    -20.00   2.40   0.70   14.00    --  -18.72 -57.00  30.00   32
 12  ω    -44.00  18.30   0.70   14.00    --  -18.72  39.00 -12.00   89
 13  ω      4.00  39.00   0.70   14.00    --   17.94 -57.00  30.00   50
 14  ω     -3.00  19.40   0.70   14.00    --   17.94  57.00 150.00   32
 15  ω    -12.70   9.00   0.70   14.00    --   17.94  77.00 -60.00   31
 16  ω    -26.00  17.40   0.70   14.00    --   17.94  19.00-180.00   62
 17  ω      4.00  39.00   0.70   14.00    --   17.94 -57.00-150.00   50
 18  ω    -45.00 -25.40   0.70   14.00    --  -18.72  37.00   0.00   28
 19  ω    -19.00   5.50   0.70   14.00    --  -18.72 -39.00-167.00   35
 20  ω    -43.00   8.10   0.70   14.00    --  -18.72  67.00 157.00   73
 21  ω    -43.00 -11.50   0.70   14.00    --  -18.72  19.00   0.00   45
 22  ω    -19.00   5.50   0.70   14.00    --  -18.72 -39.00  12.00   35
 23  ω    -36.00  26.30   0.70   14.00    --   17.94  13.00 176.00   89
 24  ω    -27.00  35.30   0.70   14.00    --   17.94 -13.00-176.00   89
 25  ω    -19.00  43.30   0.70   14.00    --   17.94 -19.00-180.00   89
 26  ω      9.00  52.40   0.70   14.00    --   17.94 -99.00  30.00   62
 27  ω    -23.00  39.30   0.70   14.00    --   17.94 -26.00   7.00   89
 28  ω    -23.00  39.30   0.70   14.00    --   17.94 -26.00-172.00   89
 29  ω    -59.00  -4.40   0.70   14.00    --  -18.72  97.00 143.00   78
 30  ω    -27.00  35.30   0.70   14.00    --  -18.72 -13.00   3.00   89
 31  ω    -44.00  18.30   0.70   14.00    --  -18.72  19.00-180.00   89
 32  ω    -40.00  13.20   0.70   14.00    --  -18.72  53.00 -17.00   76
 33  ω    -40.00  22.30   0.70   14.00    --  -18.72  26.00  -7.00   89
 34  ω    -44.00  18.30   0.70   14.00    --  -18.72  39.00 -12.00   89
 35  ω    -27.00  -1.80   0.70   14.00    --  -18.72 -13.00-176.00   36
 36  ω    -36.00  26.30   0.70   14.00    --  -18.72  13.00  -3.00   89
;
_diffrn_measurement_method       'ω scans'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                296
_reflns_number_total             537
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.967
_refine_diff_density_min         -0.654
_refine_diff_density_rms         0.197
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         537
_refine_ls_number_restraints     211
_refine_ls_R_factor_all          0.1508
_refine_ls_R_factor_gt           0.0732
_refine_ls_restrained_S_all      0.816
_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)+(0.1142P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1562
_refine_ls_wR_factor_ref         0.1948
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 C3-C2
 2.1 with sigma of 0.02
3. Rigid bond restraints
 N3, C4, C6, N4, C5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Br2, Br1, Br3, Pb1, Br4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N1, C2, N2, C3, C1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C5 \\sim N4 \\sim C6 \\sim C4 \\sim N3: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Br4 \\sim Pb1 \\sim Br3 \\sim Br1 \\sim Br2: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C2 \\sim N2 \\sim C3 \\sim C1 \\sim N1: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Uanis(N3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(N4) \\sim
Ueq, Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(Br4) \\sim Ueq, Uanis(Pb1) \\sim Ueq, Uanis(Br3) \\sim Ueq, Uanis(Br1)
\\sim Ueq, Uanis(Br2) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(N1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C3) \\sim
Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
5. Rigid body (RIGU) restrains
 C5, N4, C6, C4, N3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a :
 C2(N2,C3,C1,N1), C4(N3,C5,N4,C6)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), N2(H2A), C3(H3), C1(H1), N1(H1A), C4(H4), N3(H3A), C5(H5), N4(H4A),
 C6(H6)
;
_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 0.5641(4) 0.5776(2) 0.3167(6) 0.058(4) Uani 1 1 d . U . . .
Br1 Br 0.5113(9) 0.7241(6) 0.4991(16) 0.055(4) Uani 1 1 d . U . . .
Br2 Br 0.0684(8) 0.5992(6) 0.3450(15) 0.050(4) Uani 1 1 d . U . . .
Br3 Br 0.5327(9) 0.8916(6) 0.1643(16) 0.058(5) Uani 1 1 d . U . . .
Br4 Br 0.5220(9) 0.3843(6) 0.1566(17) 0.058(4) Uani 1 1 d . U . . .
C2 C 1.001(7) 0.627(4) 0.085(7) 0.076(12) Uani 1 1 d DG U . . .
H2 H 1.031972 0.532520 0.140444 0.091 Uiso 1 1 calc R U . . .
N2 N 1.115(8) 0.757(5) 0.066(8) 0.080(12) Uani 1 1 d G U . . .
H2A H 1.226802 0.769835 0.101410 0.096 Uiso 1 1 calc R U . . .
C3 C 1.019(8) 0.860(4) -0.018(8) 0.078(12) Uani 1 1 d DG U . . .
H3 H 1.060545 0.963085 -0.051405 0.094 Uiso 1 1 calc R U . . .
C1 C 0.844(8) 0.793(5) -0.052(8) 0.078(12) Uani 1 1 d G U . . .
H1 H 0.751213 0.844011 -0.110348 0.094 Uiso 1 1 calc R U . . .
N1 N 0.833(8) 0.649(4) 0.012(8) 0.071(11) Uani 1 1 d G U . . .
H1A H 0.740220 0.581577 0.008970 0.085 Uiso 1 1 calc R U . . .
C4 C 0.056(7) 0.181(4) 0.358(9) 0.052(9) Uani 1 1 d G U . . .
H4 H 0.083631 0.277365 0.364904 0.062 Uiso 1 1 calc R U . . .
N3 N -0.128(7) 0.144(4) 0.327(9) 0.055(9) Uani 1 1 d G U . . .
H3A H -0.249491 0.205478 0.308795 0.066 Uiso 1 1 calc R U . . .
C5 C -0.106(8) -0.001(4) 0.327(9) 0.054(9) Uani 1 1 d G U . . .
H5 H -0.215075 -0.054867 0.308209 0.065 Uiso 1 1 calc R U . . .
N4 N 0.093(7) -0.053(4) 0.358(8) 0.052(9) Uani 1 1 d G U . . .
H4A H 0.152472 -0.145430 0.365707 0.063 Uiso 1 1 calc R U . . .
C6 C 0.193(7) 0.060(4) 0.377(10) 0.049(9) Uani 1 1 d G U . . .
H6 H 0.340903 0.051908 0.401071 0.059 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 2.949(10) 2_666 ?
Pb1 Br1 2.91(2) . ?
Pb1 Br2 2.995(6) 1_655 ?
Pb1 Br2 2.805(5) . ?
Pb1 Br3 2.864(9) . ?
Pb1 Br4 3.06(2) . ?
C2 H2 0.9300 . ?
C2 N2 1.341(13) . ?
C2 N1 1.368(14) . ?
N2 H2A 0.8600 . ?
N2 C3 1.305(13) . ?
C3 H3 0.9300 . ?
C3 C1 1.389(14) . ?
C1 H1 0.9300 . ?
C1 N1 1.289(13) . ?
N1 H1A 0.8600 . ?
C4 H4 0.9300 . ?
C4 N3 1.28(3) . ?
C4 C6 1.27(3) . ?
N3 H3A 0.8600 . ?
N3 C5 1.30(3) . ?
C5 H5 0.9300 . ?
C5 N4 1.26(3) . ?
N4 H4A 0.8600 . ?
N4 C6 1.31(3) . ?
C6 H6 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br1 Pb1 Br1 88.0(3) . 2_666 ?
Br1 Pb1 Br2 96.0(3) 2_666 1_655 ?
Br1 Pb1 Br2 78.2(4) . 1_655 ?
Br1 Pb1 Br4 82.9(4) 2_666 . ?
Br1 Pb1 Br4 167.1(2) . . ?
Br2 Pb1 Br1 84.2(4) . . ?
Br2 Pb1 Br1 83.0(2) . 2_666 ?
Br2 Pb1 Br2 162.4(7) . 1_655 ?
Br2 Pb1 Br3 85.1(2) . . ?
Br2 Pb1 Br4 111.7(4) 1_655 . ?
Br2 Pb1 Br4 85.7(4) . . ?
Br3 Pb1 Br1 84.2(4) . . ?
Br3 Pb1 Br1 166.4(4) . 2_666 ?
Br3 Pb1 Br2 93.3(2) . 1_655 ?
Br3 Pb1 Br4 102.8(5) . . ?
Pb1 Br1 Pb1 92.0(3) . 2_666 ?
Pb1 Br2 Pb1 162.4(7) . 1_455 ?
N2 C2 H2 123.9 . . ?
N2 C2 N1 112.2 . . ?
N1 C2 H2 123.9 . . ?
C2 N2 H2A 128.1 . . ?
C3 N2 C2 103.9 . . ?
C3 N2 H2A 128.1 . . ?
N2 C3 H3 124.8 . . ?
N2 C3 C1 110.5 . . ?
C1 C3 H3 124.8 . . ?
C3 C1 H1 125.9 . . ?
N1 C1 C3 108.2 . . ?
N1 C1 H1 125.9 . . ?
C2 N1 H1A 127.4 . . ?
C1 N1 C2 105.3 . . ?
C1 N1 H1A 127.4 . . ?
N3 C4 H4 127.3 . . ?
C6 C4 H4 127.3 . . ?
C6 C4 N3 105.5 . . ?
C4 N3 H3A 124.8 . . ?
C4 N3 C5 110.3 . . ?
C5 N3 H3A 124.8 . . ?
N3 C5 H5 126.6 . . ?
N4 C5 N3 106.7 . . ?
N4 C5 H5 126.6 . . ?
C5 N4 H4A 126.1 . . ?
C5 N4 C6 107.8 . . ?
C6 N4 H4A 126.1 . . ?
C4 C6 N4 109.7 . . ?
C4 C6 H6 125.2 . . ?
N4 C6 H6 125.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 N2 C3 C1 0.0 . . . . ?
N2 C2 N1 C1 0.0 . . . . ?
N2 C3 C1 N1 0.0 . . . . ?
C3 C1 N1 C2 0.0 . . . . ?
N1 C2 N2 C3 0.0 . . . . ?
C4 N3 C5 N4 -0.1 . . . . ?
N3 C4 C6 N4 -0.1 . . . . ?
N3 C5 N4 C6 0.0 . . . . ?
C5 N4 C6 C4 0.0 . . . . ?
C6 C4 N3 C5 0.1 . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'

# end
####################################################################### 
# 
# 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_im3pbbr5_297gpa
_database_code_depnum_ccdc_archive 'CCDC 2473984'
loop_
_audit_author_name
_audit_author_address
'Kinga Roszak'
;Adam Mickiewicz University Poznan
Poland
;
_audit_update_record             
;
2025-07-18 deposited with the CCDC.	2026-03-26 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_im3pbbr5_297gpa     
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.242 Why?  
RESPONSE: The data come from high-pressure studies and are 
limited by the DAC opening angle.
;
_vrf_PLAT090_im3pbbr5_297gpa     
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       2.33 Note  
RESPONSE:  The data/parameter ratio is affected by the access limits of the DAC.
;
_vrf_PLAT342_im3pbbr5_297gpa     
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............       0.14 Ang.  
RESPONSE: Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the X-ray 
radiation to the measured sample
;
_vrf_PLAT031_im3pbbr5_297gpa     
;
PROBLEM: Refined Extinction Parameter Within Range of ...      1.667 Sigma 
RESPONSE: Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the X-ray 
radiation to the measured sample
;
_vrf_PLAT910_im3pbbr5_297gpa     
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         12 Note  
RESPONSE: These reflections were probably affected 
by unexpected deviations in their intensities for symmetry 
equivalent measurements and omitted during initial data reduction.
;
_vrf_PLAT911_im3pbbr5_297gpa     
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        847 Report
RESPONSE: These reflections were probably affected 
by unexpected deviations in their intensities for symmetry 
equivalent measurements and omitted during initial data reduction.
;
_vrf_PLAT915_im3pbbr5_297gpa     
;
PROBLEM: No Flack x Check Done: Low Friedel Pair Coverage         21 %     
RESPONSE: Because the Friedel Pair Coverage was low the absolute configuration was
assigned using the known absolute configuration of the molecules
;
_vrf_PLAT987_im3pbbr5_297gpa     
;
PROBLEM: The Flack x is >> 0 -  Do a BASF/TWIN Refinement     Please Check 
RESPONSE: As indicated by the Flack
parameter, the structures were refined as twins. 
All refinements converged to the racemic-twin compounds.
;
# end Validation Reply Form

_audit_creation_date             2025-04-14
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br5 Pb, 3(C3 H5 N2)'
_chemical_formula_sum            'C9 H15 Br5 N6 Pb'
_chemical_formula_weight         814.01
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   5.8382(4)
_cell_length_b                   9.0575(19)
_cell_length_c                   8.999(3)
_cell_angle_alpha                65.44(3)
_cell_angle_beta                 83.329(15)
_cell_angle_gamma                86.199(13)
_cell_volume                     429.8(2)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    1207
_cell_measurement_pressure       2970000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.5930
_cell_measurement_theta_min      4.6820
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    21.437
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.10913
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.89a (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_density_diffrn    3.145
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             368
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_av_unetI/netI     0.0532
_diffrn_reflns_Laue_measured_fraction_full 0.239
_diffrn_reflns_Laue_measured_fraction_max 0.221
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            2167
_diffrn_reflns_point_group_measured_fraction_full 0.239
_diffrn_reflns_point_group_measured_fraction_max 0.221
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.401
_diffrn_reflns_theta_min         4.660
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2413
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.242
_diffrn_measured_fraction_theta_max 0.224
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  19.75   0.75   30.00   0.00 -30.00   0.00    --    73
  2  φ    140.00 200.00   0.75   30.00   0.00 -30.00   0.00    --    80
  3  φ    160.00 217.00   0.75   30.00   0.00  30.00   0.00    --    76
  4  φ    -20.00  34.75   0.75   30.00   0.00  30.00   0.00    --    73
  5  ω    -24.00  24.00   0.75   30.00    --   30.00  39.46 -12.90   64
  6  ω    -24.00  24.00   0.75   30.00    --   30.00  39.46 167.10   64
  7  ω    -50.00  10.00   0.75   30.00    --  -30.00  39.46 167.10   80
  8  ω    -50.00  10.00   0.75   30.00    --  -30.00  39.46 -12.90   80
  9  ω    -64.00  -8.50   0.75   30.00    --  -30.00  81.40 -28.90   74
 10  ω    -64.00  -8.50   0.75   30.00    --  -30.00  81.40 151.10   74
 11  ω    -19.00   8.00   0.75   30.00    --   30.00  81.40 151.10   36
 12  ω    -19.00   8.00   0.75   30.00    --   30.00  81.40 -28.90   36
 13  ω    -43.00 -21.25   0.75   30.00    --   30.00 134.60 -56.90   29
 14  ω    -43.00 -21.25   0.75   30.00    --   30.00 134.60 123.10   29
 15  ω    -90.00 -36.00   0.75   30.00    --  -30.00 134.60 123.10   72
 16  ω    -90.00 -36.00   0.75   30.00    --  -30.00 134.60 -56.90   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_axis[1]    matrixX
_diffrn_orient_matrix_axis[2]    matrixY
_diffrn_orient_matrix_axis[3]    matrixZ
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0147459496
_diffrn_orient_matrix_UB_12      -0.0449581585
_diffrn_orient_matrix_UB_13      0.0875162995
_diffrn_orient_matrix_UB_21      -0.1209383350
_diffrn_orient_matrix_UB_22      0.0138822245
_diffrn_orient_matrix_UB_23      -0.0009055559
_diffrn_orient_matrix_UB_31      -0.0111730892
_diffrn_orient_matrix_UB_32      -0.0721288138
_diffrn_orient_matrix_UB_33      -0.0113468229
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.239
_reflns_Friedel_fraction_max     0.221
_reflns_number_gt                697
_reflns_number_total             759
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXD  (Sheldrick, 2008)'
_refine_diff_density_max         0.694
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.121
_refine_ls_abs_structure_details 
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack   0.5
_refine_ls_extinction_coef       0.005(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         759
_refine_ls_number_restraints     245
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0393
_refine_ls_restrained_S_all      0.916
_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)+(0.0486P)²+6.3359P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0916
_refine_ls_wR_factor_ref         0.0944
_refine_special_details          
;
 Refined as a 2-component perfect inversion twin.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 C5-C4
 1.28 with sigma of 0.02
 C9-C8
 2.1 with sigma of 0.02
3. Rigid bond restraints
 N3, C6, N4, C5, C4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N2, C1, N1, C2, C3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N6, C9, N5, C8, C7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Br3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Br5, Br2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C5 \\sim N4 \\sim N3 \\sim C6 \\sim C4: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
C3 \\sim C2 \\sim N1 \\sim C1 \\sim N2: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
C9 \\sim N5 \\sim C8 \\sim C7 \\sim N6: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Br3: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Br2 \\sim Br5: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
Uanis(C9) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C7) \\sim
Ueq, Uanis(N6) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of
0.008
Uanis(C5) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C6) \\sim
Ueq, Uanis(N4) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of
0.008
Uanis(C3) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C1) \\sim
Ueq, Uanis(N2) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of
0.008
Uanis(Br3) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(Br5) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(Br2) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(C9) \\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim
Ueq, Uanis(N5) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of
0.008
Uanis(Br1) \\sim Ueq, Uanis(Br4) \\sim Ueq: with sigma of 0.004 and sigma for
terminal atoms of 0.008
5.a :
 C3(N2,C1,N1,C2), N3(C6,N4,C5,C4), C9(N5,C8,C7,N6)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), N2(H2), C1(H1), N1(H1A), C2(H2A), N3(H3A), C6(H6), N4(H4), C5(H5),
 C4(H4A), C9(H9), N5(H5A), C8(H8), C7(H7), N6(H6A)
;
_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 1.50321(18) 0.5065(2) -0.0140(3) 0.035(5) Uani 1 1 d . . . . .
Br1 Br 1.4745(14) 0.1713(17) 0.243(3) 0.041(6) Uani 1 1 d . U . . .
Br2 Br 1.5121(14) 0.3817(18) -0.278(3) 0.038(6) Uani 1 1 d . U . . .
Br3 Br 1.0064(12) 0.5343(15) -0.008(3) 0.027(3) Uani 1 1 d . U . . .
Br4 Br 1.4543(14) 0.6382(18) 0.242(3) 0.035(6) Uani 1 1 d . U . . .
Br5 Br 1.5066(14) 0.8423(19) -0.266(4) 0.038(6) Uani 1 1 d . U . . .
C3 C 0.863(7) -0.060(10) 0.966(18) 0.034(10) Uani 1 1 d G U . . .
H3 H 0.750406 -0.126738 0.962617 0.041 Uiso 1 1 calc R U . . .
N2 N 1.081(7) -0.095(9) 0.976(17) 0.028(9) Uani 1 1 d G U . . .
H2 H 1.146880 -0.183920 0.980143 0.034 Uiso 1 1 calc R U . . .
C1 C 1.184(6) 0.027(9) 0.978(19) 0.033(10) Uani 1 1 d G U . . .
H1 H 1.340587 0.033112 0.984801 0.040 Uiso 1 1 calc R U . . .
N1 N 1.030(7) 0.136(9) 0.970(18) 0.037(10) Uani 1 1 d G U . . .
H1A H 1.052555 0.229199 0.969677 0.045 Uiso 1 1 calc R U . . .
C2 C 0.831(6) 0.082(10) 0.963(19) 0.031(10) Uani 1 1 d G U . . .
H2A H 0.690329 0.138215 0.955871 0.037 Uiso 1 1 calc R U . . .
N3 N 1.123(7) 0.323(7) 0.508(14) 0.037(10) Uani 1 1 d G U . . .
H3A H 1.214636 0.400735 0.487548 0.044 Uiso 1 1 calc R U . . .
C6 C 0.938(8) 0.333(7) 0.443(14) 0.041(10) Uani 1 1 d G U . . .
H6 H 0.877031 0.426943 0.364620 0.050 Uiso 1 1 calc R U . . .
N4 N 0.848(7) 0.192(8) 0.503(14) 0.036(10) Uani 1 1 d G U . . .
H4 H 0.722259 0.168070 0.478023 0.044 Uiso 1 1 calc R U . . .
C5 C 0.979(7) 0.095(7) 0.605(13) 0.031(10) Uani 1 1 d DG U . . .
H5 H 0.955053 -0.015483 0.666661 0.038 Uiso 1 1 calc R U . . .
C4 C 1.148(7) 0.176(8) 0.608(13) 0.027(9) Uani 1 1 d DG U . . .
H4A H 1.270034 0.133523 0.672436 0.032 Uiso 1 1 calc R U . . .
C9 C 1.111(11) -0.287(12) 0.54(2) 0.082(16) Uani 1 1 d DG U . . .
H9 H 1.213863 -0.352528 0.613054 0.098 Uiso 1 1 calc R U . . .
N5 N 1.136(10) -0.134(12) 0.45(2) 0.084(16) Uani 1 1 d G U . . .
H5A H 1.249964 -0.074953 0.440217 0.101 Uiso 1 1 calc R U . . .
C8 C 0.957(13) -0.086(12) 0.36(2) 0.092(17) Uani 1 1 d DG U . . .
H8 H 0.930076 0.019016 0.286930 0.110 Uiso 1 1 calc R U . . .
C7 C 0.822(12) -0.209(13) 0.41(2) 0.086(17) Uani 1 1 d G U . . .
H7 H 0.681884 -0.207686 0.365568 0.103 Uiso 1 1 calc R U . . .
N6 N 0.916(11) -0.334(12) 0.52(2) 0.085(16) Uani 1 1 d G U . . .
H6A H 0.862032 -0.429832 0.563563 0.103 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br1 2.96(2) . ?
Pb1 Br2 3.018(19) . ?
Pb1 Br3 2.891(7) . ?
Pb1 Br3 2.973(7) 1_655 ?
Pb1 Br4 2.984(18) . ?
Pb1 Br5 2.94(2) . ?
C3 H3 0.9300 . ?
C3 N2 1.29(3) . ?
C3 C2 1.28(3) . ?
N2 H2 0.8600 . ?
N2 C1 1.30(3) . ?
C1 H1 0.9300 . ?
C1 N1 1.28(3) . ?
N1 H1A 0.8600 . ?
N1 C2 1.31(3) . ?
C2 H2A 0.9300 . ?
N3 H3A 0.8600 . ?
N3 C6 1.27(3) . ?
N3 C4 1.27(3) . ?
C6 H6 0.9300 . ?
C6 N4 1.28(3) . ?
N4 H4 0.8600 . ?
N4 C5 1.26(3) . ?
C5 H5 0.9300 . ?
C5 C4 1.28(3) . ?
C4 H4A 0.9300 . ?
C9 H9 0.9300 . ?
C9 N5 1.30(2) . ?
C9 N6 1.31(2) . ?
N5 H5A 0.8600 . ?
N5 C8 1.30(2) . ?
C8 H8 0.9300 . ?
C8 C7 1.31(2) . ?
C7 H7 0.9500 . ?
C7 N6 1.29(2) . ?
N6 H6A 0.8600 . ?

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 90.6(6) . . ?
Br1 Pb1 Br3 95.0(4) . 1_655 ?
Br1 Pb1 Br4 90.5(5) . . ?
Br3 Pb1 Br1 91.2(4) . . ?
Br3 Pb1 Br2 88.7(4) . . ?
Br3 Pb1 Br2 99.9(3) 1_655 . ?
Br3 Pb1 Br3 169.2(2) . 1_655 ?
Br3 Pb1 Br4 84.5(4) 1_655 . ?
Br3 Pb1 Br4 86.7(3) . . ?
Br3 Pb1 Br5 86.0(4) . . ?
Br4 Pb1 Br2 175.3(3) . . ?
Br5 Pb1 Br1 177.1(3) . . ?
Br5 Pb1 Br2 90.0(5) . . ?
Br5 Pb1 Br3 87.7(4) . 1_655 ?
Br5 Pb1 Br4 88.6(6) . . ?
Pb1 Br3 Pb1 169.2(2) . 1_455 ?
N2 C3 H3 126.5 . . ?
C2 C3 H3 126.5 . . ?
C2 C3 N2 106.9 . . ?
C3 N2 H2 125.4 . . ?
C3 N2 C1 109.2 . . ?
C1 N2 H2 125.4 . . ?
N2 C1 H1 126.5 . . ?
N1 C1 N2 107.1 . . ?
N1 C1 H1 126.5 . . ?
C1 N1 H1A 125.9 . . ?
C1 N1 C2 108.3 . . ?
C2 N1 H1A 125.9 . . ?
C3 C2 N1 108.5 . . ?
C3 C2 H2A 125.8 . . ?
N1 C2 H2A 125.8 . . ?
C6 N3 H3A 126.4 . . ?
C6 N3 C4 107.2 . . ?
C4 N3 H3A 126.4 . . ?
N3 C6 H6 125.7 . . ?
N3 C6 N4 108.5 . . ?
N4 C6 H6 125.7 . . ?
C6 N4 H4 126.1 . . ?
C5 N4 C6 107.9 . . ?
C5 N4 H4 126.1 . . ?
N4 C5 H5 126.2 . . ?
N4 C5 C4 107.6 . . ?
C4 C5 H5 126.2 . . ?
N3 C4 C5 108.7 . . ?
N3 C4 H4A 125.6 . . ?
C5 C4 H4A 125.6 . . ?
N5 C9 H9 125.6 . . ?
N5 C9 N6 110(11) . . ?
N6 C9 H9 125.6 . . ?
C9 N5 H5A 128.00 . . ?
C8 N5 C9 107.0 . . ?
C8 N5 H5A 125.00 . . ?
N5 C8 H8 125.6 . . ?
N5 C8 C7 107(13) . . ?
C7 C8 H8 128.00 . . ?
C8 C7 H7 124.00 . . ?
N6 C7 C8 110(9) . . ?
N6 C7 H7 126.2 . . ?
C9 N6 H6A 128.00 . . ?
C7 N6 C9 107.7 . . ?
C7 N6 H6A 125.00 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 N2 C1 N1 0.0 . . . . ?
N2 C3 C2 N1 0.0 . . . . ?
N2 C1 N1 C2 0.0 . . . . ?
C1 N1 C2 C3 0.0 . . . . ?
C2 C3 N2 C1 0.0 . . . . ?
N3 C6 N4 C5 0.0 . . . . ?
C6 N3 C4 C5 0.0 . . . . ?
C6 N4 C5 C4 0.0 . . . . ?
N4 C5 C4 N3 0.0 . . . . ?
C4 N3 C6 N4 0.0 . . . . ?
C9 N5 C8 C7 5(17) . . . . ?
N5 C9 N6 C7 3(18) . . . . ?
N5 C8 C7 N6 -4(18) . . . . ?
C8 C7 N6 C9 0.0 . . . . ?
N6 C9 N5 C8 -5(18) . . . . ?

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

data_impbbr3_063gpa
_database_code_depnum_ccdc_archive 'CCDC 2473958'
loop_
_audit_author_name
_audit_author_address
'Kinga Roszak'
;Adam Mickiewicz University Poznan
Poland
;
_audit_update_record             
;
2025-07-18 deposited with the CCDC.	2026-03-26 downloaded from the CCDC.
;
_audit_creation_date             2025-04-15
# start Validation Reply Form
_vrf_PLAT027_impbbr3_063gpa      
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      15.00 Degree
RESPONSE: A full set of data was collected, however 
the very high angle data was poor and was omitted.
Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the 
X-ray radiation to the measured sample.
;
_vrf_PLAT029_impbbr3_063gpa      
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.422 Why?  
RESPONSE: The data come from high-pressure studies and are 
limited by the DAC opening angle.
;
_vrf_PLAT090_impbbr3_063gpa      
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       3.86 Note  
RESPONSE: The data/parameter ratio is affected by the access limits of the DAC.
;
_vrf_PLAT342_impbbr3_063gpa      
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............       0.17 Ang.  
RESPONSE: Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the X-ray 
radiation to the measured sample; poor quality of measurement
;
_vrf_PLAT987_impbbr3_063gpa      
;
PROBLEM: The Flack x is >> 0 -  Do a BASF/TWIN Refinement     Please Check 
RESPONSE: The structure was refined as an inversion twin.
;
# end Validation Reply Form
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br3 Pb, C3 H5 N2'
_chemical_formula_sum            'C3 H5 Br3 N2 Pb'
_chemical_formula_weight         516.01
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, z'

_cell_length_a                   13.9667(7)
_cell_length_b                   8.759(8)
_cell_length_c                   14.8128(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1812.2(16)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    2187
_cell_measurement_pressure       630000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.6200
_cell_measurement_theta_min      4.6180
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    31.774
_exptl_absorpt_correction_T_min  0.12596
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.783
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0942
_diffrn_reflns_av_unetI/netI     0.0693
_diffrn_reflns_Laue_measured_fraction_full 0.425
_diffrn_reflns_Laue_measured_fraction_max 0.294
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       2
_diffrn_reflns_limit_k_min       -2
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7811
_diffrn_reflns_point_group_measured_fraction_full 0.432
_diffrn_reflns_point_group_measured_fraction_max 0.297
_diffrn_reflns_theta_full        15.000
_diffrn_reflns_theta_max         26.456
_diffrn_reflns_theta_min         4.638
_diffrn_ambient_temperature      293(2)
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_detector_area_resol_mean 16.2413
_diffrn_measured_fraction_theta_full 0.422
_diffrn_measured_fraction_theta_max 0.293
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0053014000
_diffrn_orient_matrix_UB_12      0.0803361000
_diffrn_orient_matrix_UB_13      0.0001093000
_diffrn_orient_matrix_UB_21      -0.0288901000
_diffrn_orient_matrix_UB_22      0.0047721000
_diffrn_orient_matrix_UB_23      0.0393412000
_diffrn_orient_matrix_UB_31      0.0415056000
_diffrn_orient_matrix_UB_32      -0.0070230000
_diffrn_orient_matrix_UB_33      0.0273937000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  19.75   0.75   35.00   0.00 -30.00   0.00    --    73
  2  φ    140.00 200.00   0.75   35.00   0.00 -30.00   0.00    --    80
  3  φ    160.00 217.00   0.75   35.00   0.00  30.00   0.00    --    76
  4  φ    -20.00  34.75   0.75   35.00   0.00  30.00   0.00    --    73
  5  ω    -24.00  24.00   0.75   35.00    --   30.00  39.46 -12.90   64
  6  ω    -24.00  24.00   0.75   35.00    --   30.00  39.46 167.10   64
  7  ω    -50.00  10.00   0.75   35.00    --  -30.00  39.46 167.10   80
  8  ω    -50.00  10.00   0.75   35.00    --  -30.00  39.46 -12.90   80
  9  ω    -64.00  -8.50   0.75   35.00    --  -30.00  81.40 -28.90   74
 10  ω    -64.00  -8.50   0.75   35.00    --  -30.00  81.40 151.10   74
 11  ω    -19.00   8.00   0.75   35.00    --   30.00  81.40 151.10   36
 12  ω    -19.00   8.00   0.75   35.00    --   30.00  81.40 -28.90   36
 13  ω    -43.00 -21.25   0.75   35.00    --   30.00 134.60 -56.90   29
 14  ω    -43.00 -21.25   0.75   35.00    --   30.00 134.60 123.10   29
 15  ω    -90.00 -36.00   0.75   35.00    --  -30.00 134.60 123.10   72
 16  ω    -90.00 -36.00   0.75   35.00    --  -30.00 134.60 -56.90   72
;
_diffrn_measurement_method       'ω and φ scans'
_reflns_Friedel_coverage         0.944
_reflns_Friedel_fraction_full    0.441
_reflns_Friedel_fraction_max     0.301
_reflns_number_gt                745
_reflns_number_total             1090
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXD  (Sheldrick, 2008)'
_refine_diff_density_max         1.010
_refine_diff_density_min         -0.985
_refine_diff_density_rms         0.247
_refine_ls_abs_structure_details 
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack   0.5
_refine_ls_extinction_coef       0.0010(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         1090
_refine_ls_number_restraints     165
_refine_ls_R_factor_all          0.0856
_refine_ls_R_factor_gt           0.0467
_refine_ls_restrained_S_all      0.924
_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)+(0.0826P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1147
_refine_ls_wR_factor_ref         0.1397
_refine_special_details          
;
 Refined as a 2-component perfect inversion twin.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Rigid bond restraints
 C4, N3, C6, C5, N4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C3, N2, C2, N1, C1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Br1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Br5, Br3, Br6, Br2, Br4, Br1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
N3 \\sim C6 \\sim C5 \\sim N4 \\sim C4: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
N2 \\sim C2 \\sim N1 \\sim C1 \\sim C3: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
C3 \\sim N2 \\sim C2 \\sim N1 \\sim C1: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Br1: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Br3 \\sim Br6 \\sim Br4 \\sim Br2 \\sim Br5 \\sim Br1: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(Br1) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(N3) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(N4) \\sim
Ueq, Uanis(C4) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of
0.008
Uanis(C3) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C2) \\sim
Ueq, Uanis(N2) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of
0.008
Uanis(Pb2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(Br3) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(Br5) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4.a :
 C3(C1,N1,C2,N2), C6(C5,N4,C4,N3)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C1(H1), N1(H1A), C2(H2), N2(H2A), C6(H6), C5(H5), N4(H4), C4(H4A),
 N3(H3A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.1724(5) 0.013(2) 0.36656(10) 0.034(7) Uani 1 1 d . . . . .
Pb2 Pb 0.1728(5) 0.0153(19) 0.62768(11) 0.0303(17) Uani 1 1 d . U . . .
Br1 Br 0.2322(13) 0.284(8) 0.2581(9) 0.054(6) Uani 1 1 d . U . . .
Br2 Br 0.0669(3) 0.2080(18) 0.4979(12) 0.050(11) Uani 1 1 d . . . . .
Br3 Br -0.0015(17) -0.001(5) 0.7428(11) 0.0380(19) Uani 1 1 d . U . . .
Br4 Br 0.3339(3) 0.0545(17) 0.4959(16) 0.041(11) Uani 1 1 d . . . . .
Br5 Br 0.1185(3) -0.2379(19) 0.4974(13) 0.0486(16) Uani 1 1 d . U . . .
Br6 Br 0.2347(12) 0.287(7) 0.7389(8) 0.048(15) Uani 1 1 d . . . . .
C3 C 0.369(5) 0.634(12) 0.449(8) 0.066(12) Uani 1 1 d G U . . .
H3 H 0.396051 0.707543 0.411688 0.079 Uiso 1 1 calc R U . . .
C1 C 0.377(4) 0.626(11) 0.537(8) 0.066(12) Uani 1 1 d G U . . .
H1 H 0.410613 0.694353 0.573499 0.079 Uiso 1 1 calc R U . . .
N1 N 0.329(7) 0.506(15) 0.565(7) 0.067(12) Uani 1 1 d G U . . .
H1A H 0.322920 0.476539 0.620200 0.080 Uiso 1 1 calc R U . . .
C2 C 0.291(2) 0.439(10) 0.494(9) 0.066(11) Uani 1 1 d G U . . .
H2 H 0.253246 0.351282 0.494612 0.080 Uiso 1 1 calc R U . . .
N2 N 0.316(6) 0.518(15) 0.422(7) 0.066(12) Uani 1 1 d G U . . .
H2A H 0.300162 0.497153 0.367389 0.080 Uiso 1 1 calc R U . . .
C6 C 0.476(5) 0.110(16) 0.299(4) 0.047(12) Uani 1 1 d G U . . .
H6 H 0.455970 0.179417 0.342615 0.057 Uiso 1 1 calc R U . . .
C5 C 0.528(5) -0.006(17) 0.312(4) 0.052(12) Uani 1 1 d G U . . .
H5 H 0.553360 -0.037334 0.366533 0.062 Uiso 1 1 calc R U . . .
N4 N 0.540(4) -0.075(15) 0.232(5) 0.059(12) Uani 1 1 d G U . . .
H4 H 0.573337 -0.156702 0.223701 0.071 Uiso 1 1 calc R U . . .
C4 C 0.496(5) -0.003(15) 0.170(3) 0.052(12) Uani 1 1 d G U . . .
H4A H 0.492942 -0.026143 0.109171 0.063 Uiso 1 1 calc R U . . .
N3 N 0.457(3) 0.112(14) 0.212(5) 0.052(11) Uani 1 1 d G U . . .
H3A H 0.421856 0.179872 0.186035 0.062 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 2.98(6) . ?
Pb1 Br2 2.98(2) . ?
Pb1 Br3 3.01(2) 2_554 ?
Pb1 Br4 2.981(17) . ?
Pb1 Br5 3.03(2) . ?
Pb1 Br6 3.03(4) 3_544 ?
Pb2 Br1 3.10(5) 3_545 ?
Pb2 Br2 2.955(19) . ?
Pb2 Br3 2.97(2) . ?
Pb2 Br4 2.999(17) . ?
Pb2 Br5 3.04(2) . ?
Pb2 Br6 3.02(5) . ?
C3 H3 0.9300 . ?
C3 C1 1.31(4) . ?
C3 N2 1.32(4) . ?
C1 H1 0.9300 . ?
C1 N1 1.32(4) . ?
N1 H1A 0.8600 . ?
N1 C2 1.32(4) . ?
C2 H2 0.9300 . ?
C2 N2 1.32(4) . ?
N2 H2A 0.8600 . ?
C6 H6 0.9300 . ?
C6 C5 1.26(3) . ?
C6 N3 1.32(4) . ?
C5 H5 0.9300 . ?
C5 N4 1.34(4) . ?
N4 H4 0.8600 . ?
N4 C4 1.27(4) . ?
C4 H4A 0.9300 . ?
C4 N3 1.30(4) . ?
N3 H3A 0.8600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br1 Pb1 Br3 85.6(8) . 2_554 ?
Br1 Pb1 Br5 172.8(8) . . ?
Br1 Pb1 Br6 93.7(16) . 3_544 ?
Br2 Pb1 Br1 92.0(9) . . ?
Br2 Pb1 Br3 91.5(7) . 2_554 ?
Br2 Pb1 Br4 83.4(5) . . ?
Br2 Pb1 Br5 82.8(5) . . ?
Br2 Pb1 Br6 173.7(11) . 3_544 ?
Br3 Pb1 Br5 99.5(8) 2_554 . ?
Br3 Pb1 Br6 86.3(8) 2_554 3_544 ?
Br4 Pb1 Br1 92.2(6) . . ?
Br4 Pb1 Br3 174.4(11) . 2_554 ?
Br4 Pb1 Br5 82.2(5) . . ?
Br4 Pb1 Br6 99.0(5) . 3_544 ?
Br5 Pb1 Br6 91.8(10) . 3_544 ?
Br2 Pb2 Br1 173.6(11) . 3_545 ?
Br2 Pb2 Br3 89.4(7) . . ?
Br2 Pb2 Br4 83.5(4) . . ?
Br2 Pb2 Br5 83.0(5) . . ?
Br2 Pb2 Br6 92.7(8) . . ?
Br3 Pb2 Br1 87.9(8) . 3_545 ?
Br3 Pb2 Br4 172.9(7) . . ?
Br3 Pb2 Br5 97.2(8) . . ?
Br3 Pb2 Br6 87.6(8) . . ?
Br4 Pb2 Br1 99.2(4) . 3_545 ?
Br4 Pb2 Br5 81.8(4) . . ?
Br4 Pb2 Br6 92.8(5) . . ?
Br5 Pb2 Br1 91.5(11) . 3_545 ?
Br6 Pb2 Br1 93.0(16) . 3_545 ?
Br6 Pb2 Br5 173.5(7) . . ?
Pb1 Br1 Pb2 167.2(16) . 3_554 ?
Pb2 Br2 Pb1 81.4(3) . . ?
Pb2 Br3 Pb1 177.4(8) . 2 ?
Pb1 Br4 Pb2 80.60(11) . . ?
Pb1 Br5 Pb2 79.3(4) . . ?
Pb2 Br6 Pb1 167.9(15) . 3 ?
C1 C3 H3 126.0 . . ?
C1 C3 N2 108.0 . . ?
N2 C3 H3 126.0 . . ?
C3 C1 H1 126.0 . . ?
C3 C1 N1 107.92(5) . . ?
N1 C1 H1 126.0 . . ?
C1 N1 H1A 125.9 . . ?
C2 N1 C1 108.2 . . ?
C2 N1 H1A 125.9 . . ?
N1 C2 H2 126.1 . . ?
N1 C2 N2 107.8 . . ?
N2 C2 H2 126.1 . . ?
C3 N2 H2A 125.9 . . ?
C2 N2 C3 108.1 . . ?
C2 N2 H2A 125.9 . . ?
C5 C6 H6 126.00 . . ?
C5 C6 N3 105.8 . . ?
N3 C6 H6 127.1 . . ?
C6 C5 H5 125.9 . . ?
C6 C5 N4 107(7) . . ?
N4 C5 H5 125.9 . . ?
C5 N4 H4 124.9 . . ?
C4 N4 C5 110.1 . . ?
C4 N4 H4 124.9 . . ?
N4 C4 H4A 127.8 . . ?
N4 C4 N3 104.5 . . ?
N3 C4 H4A 127.8 . . ?
C6 N3 H3A 124.3 . . ?
C4 N3 C6 111.5 . . ?
C4 N3 H3A 124.3 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 C1 N1 C2 0.0 . . . . ?
C1 C3 N2 C2 0.0 . . . . ?
C1 N1 C2 N2 0.1 . . . . ?
N1 C2 N2 C3 0.0 . . . . ?
N2 C3 C1 N1 0.0 . . . . ?
C6 C5 N4 C4 0.0 . . . . ?
C5 C6 N3 C4 0.0 . . . . ?
C5 N4 C4 N3 0.0 . . . . ?
N4 C4 N3 C6 0.0 . . . . ?
N3 C6 C5 N4 0.0 . . . . ?

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

data_impbbr3_306gpa
_database_code_depnum_ccdc_archive 'CCDC 2473965'
loop_
_audit_author_name
_audit_author_address
'Kinga Roszak'
;Adam Mickiewicz University Poznan
Poland
;
_audit_update_record             
;
2025-07-18 deposited with the CCDC.	2026-03-26 downloaded from the CCDC.
;
_audit_creation_date             2024-08-01
# start Validation Reply Form
_vrf_PLAT027_impbbr3_306gpa      
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      17.50 Degree
RESPONSE: A full set of data was collected, however 
the very high angle data was poor and was omitted.
Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the 
X-ray radiation to the measured sample.
;
_vrf_PLAT029_impbbr3_306gpa      
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.503 Why?  
RESPONSE: The data come from high-pressure studies and are 
limited by the DAC opening angle.
;
_vrf_PLAT090_impbbr3_306gpa      
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       4.39 Note  
RESPONSE: The data/parameter ratio is affected by the access limits of the DAC.
;
_vrf_PLAT342_impbbr3_306gpa      
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............      0.055 Ang.  
RESPONSE: Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the X-ray 
radiation to the measured sample; poor quality of measurement
;
_vrf_PLAT911_impbbr3_306gpa      
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        333 Report
RESPONSE: These reflections were probably affected 
by unexpected deviations in their intensities for symmetry 
equivalent measurements and omitted during initial data reduction.
;
_vrf_PLAT987_impbbr3_306gpa      
;
PROBLEM: The Flack x is >> 0 -  Do a BASF/TWIN Refinement     Please Check 
RESPONSE: The structure was refined as an inversion twin.
;
# end Validation Reply Form
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br3 Pb, C3 H5 N2'
_chemical_formula_sum            'C3 H5 Br3 N2 Pb'
_chemical_formula_weight         516.01
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z+1/2'

_cell_length_a                   13.2201(7)
_cell_length_b                   8.379(3)
_cell_length_c                   14.4383(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1599.3(6)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    1947
_cell_measurement_pressure       3060000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.6090
_cell_measurement_theta_min      4.1640
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    36.003
_exptl_absorpt_correction_T_min  0.41921
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    4.286
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0884
_diffrn_reflns_av_unetI/netI     0.0717
_diffrn_reflns_Laue_measured_fraction_full 0.503
_diffrn_reflns_Laue_measured_fraction_max 0.361
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7182
_diffrn_reflns_point_group_measured_fraction_full 0.509
_diffrn_reflns_point_group_measured_fraction_max 0.364
_diffrn_reflns_theta_full        17.500
_diffrn_reflns_theta_max         26.891
_diffrn_reflns_theta_min         4.173
_diffrn_ambient_temperature      293(2)
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_detector_area_resol_mean 16.1544
_diffrn_measured_fraction_theta_full 0.503
_diffrn_measured_fraction_theta_max 0.361
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0157890181
_diffrn_orient_matrix_UB_12      0.0808646787
_diffrn_orient_matrix_UB_13      0.0000089882
_diffrn_orient_matrix_UB_21      0.0325357929
_diffrn_orient_matrix_UB_22      0.0157313368
_diffrn_orient_matrix_UB_23      -0.0379997076
_diffrn_orient_matrix_UB_31      -0.0396629703
_diffrn_orient_matrix_UB_32      -0.0192792336
_diffrn_orient_matrix_UB_33      -0.0311458742
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  19.75   0.75   27.00   0.00 -30.00   0.00    --    73
  2  φ    140.00 200.00   0.75   27.00   0.00 -30.00   0.00    --    80
  3  φ    160.00 217.00   0.75   27.00   0.00  30.00   0.00    --    76
  4  φ    -20.00  34.75   0.75   27.00   0.00  30.00   0.00    --    73
  5  ω    -24.00  24.00   0.75   27.00    --   30.00  39.46 -12.90   64
  6  ω    -24.00  24.00   0.75   27.00    --   30.00  39.46 167.10   64
  7  ω    -50.00  10.00   0.75   27.00    --  -30.00  39.46 167.10   80
  8  ω    -50.00  10.00   0.75   27.00    --  -30.00  39.46 -12.90   80
  9  ω    -64.00  -8.50   0.75   27.00    --  -30.00  81.40 -28.90   74
 10  ω    -64.00  -8.50   0.75   27.00    --  -30.00  81.40 151.10   74
 11  ω    -19.00   8.00   0.75   27.00    --   30.00  81.40 151.10   36
 12  ω    -19.00   8.00   0.75   27.00    --   30.00  81.40 -28.90   36
 13  ω    -43.00 -21.25   0.75   27.00    --   30.00 134.60 -56.90   29
 14  ω    -43.00 -21.25   0.75   27.00    --   30.00 134.60 123.10   29
 15  ω    -90.00 -36.00   0.75   27.00    --  -30.00 134.60 123.10   72
 16  ω    -90.00 -36.00   0.75   27.00    --  -30.00 134.60 -56.90   72
;
_diffrn_measurement_method       'ω and φ scans'
_reflns_Friedel_coverage         0.934
_reflns_Friedel_fraction_full    0.517
_reflns_Friedel_fraction_max     0.366
_reflns_number_gt                932
_reflns_number_total             1220
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.794
_refine_diff_density_min         -0.781
_refine_diff_density_rms         0.203
_refine_ls_abs_structure_details 
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack   0.5
_refine_ls_extinction_coef       0.00086(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         1220
_refine_ls_number_restraints     118
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0412
_refine_ls_restrained_S_all      0.987
_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)+(0.0293P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0718
_refine_ls_wR_factor_ref         0.0797
_refine_special_details          
;
 Refined as a 2-component perfect inversion twin.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 C6-C5
 1.35 with sigma of 0.02
3. Rigid bond restraints
 C1, N1, C2, N2, C3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C6, C5, N3, C4, N4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C3 \\sim N2 \\sim C2 \\sim N1 \\sim C1: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
C5 \\sim N4 \\sim C4 \\sim N3 \\sim C6: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Uanis(N2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(N1) \\sim
Ueq, Uanis(C2) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of
0.008
Uanis(C6) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
5.a :
 C3(C1,N1,C2,N2), C5(N4,C4,N3,C6)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C1(H1), N1(H1A), C2(H2), N2(H2A), C5(H5), N4(H4), C4(H4A), N3(H3A),
 C6(H6)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.16770(12) -0.0055(5) 0.36793(9) 0.0213(18) Uani 1 1 d . . . . .
Pb2 Pb 0.18496(10) 0.0072(5) 0.62619(9) 0.0229(18) Uani 1 1 d . . . . .
Br1 Br 0.2301(3) 0.2690(15) 0.2596(3) 0.030(5) Uani 1 1 d . . . . .
Br2 Br 0.0625(3) 0.2045(11) 0.4996(4) 0.030(5) Uani 1 1 d . . . . .
Br3 Br 0.0074(3) -0.0150(13) 0.7389(4) 0.022(5) Uani 1 1 d . . . . .
Br4 Br 0.3451(3) 0.0472(11) 0.4792(3) 0.032(5) Uani 1 1 d . . . . .
Br5 Br 0.1233(3) -0.2659(12) 0.5093(3) 0.028(4) Uani 1 1 d . . . . .
Br6 Br 0.2139(3) 0.3033(14) 0.7354(3) 0.024(6) Uani 1 1 d . . . . .
C3 C 0.2916(19) 0.438(5) 0.491(3) 0.032(8) Uani 1 1 d G U . . .
H3 H 0.250254 0.348153 0.488711 0.039 Uiso 1 1 calc R U . . .
C1 C 0.329(2) 0.514(6) 0.419(2) 0.028(8) Uani 1 1 d G U . . .
H1 H 0.318834 0.487047 0.356841 0.034 Uiso 1 1 calc R U . . .
N1 N 0.3835(19) 0.634(5) 0.449(3) 0.039(8) Uani 1 1 d G U . . .
H1A H 0.415907 0.701693 0.415913 0.047 Uiso 1 1 calc R U . . .
C2 C 0.3797(19) 0.632(5) 0.540(2) 0.030(8) Uani 1 1 d G U . . .
H2 H 0.411514 0.704451 0.579883 0.036 Uiso 1 1 calc R U . . .
N2 N 0.323(2) 0.511(6) 0.566(2) 0.030(7) Uani 1 1 d G U . . .
H2A H 0.308695 0.484668 0.621986 0.036 Uiso 1 1 calc R U . . .
C5 C 0.562(2) -0.080(6) 0.291(2) 0.042(14) Uani 1 1 d DG U . . .
H5 H 0.598904 -0.136806 0.335163 0.051 Uiso 1 1 calc R U . . .
N4 N 0.552(2) -0.118(7) 0.201(2) 0.053(15) Uani 1 1 d G U . . .
H4 H 0.578008 -0.199449 0.173868 0.064 Uiso 1 1 calc R U . . .
C4 C 0.493(2) -0.006(7) 0.1608(19) 0.045(17) Uani 1 1 d G U . . .
H4A H 0.473302 -0.003786 0.098898 0.054 Uiso 1 1 calc R U . . .
N3 N 0.466(2) 0.101(7) 0.226(2) 0.055(15) Uani 1 1 d G U . . .
H3A H 0.428997 0.183767 0.218119 0.066 Uiso 1 1 calc R U . . .
C6 C 0.509(3) 0.056(6) 0.3070(19) 0.027(10) Uani 1 1 d DG U . . .
H6 H 0.503552 0.108286 0.363478 0.032 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 2.901(11) . ?
Pb1 Br2 2.940(8) . ?
Pb1 Br3 2.977(5) 2_554 ?
Pb1 Br4 2.876(5) . ?
Pb1 Br5 3.045(9) . ?
Pb1 Br6 2.946(8) 4_544 ?
Pb2 Br1 2.992(10) 4_545 ?
Pb2 Br2 2.949(7) . ?
Pb2 Br3 2.862(5) . ?
Pb2 Br4 3.017(4) . ?
Pb2 Br5 2.958(9) . ?
Pb2 Br6 2.964(11) . ?
C3 H3 0.9300 . ?
C3 C1 1.32(2) . ?
C3 N2 1.32(2) . ?
C1 H1 0.9300 . ?
C1 N1 1.32(2) . ?
N1 H1A 0.8600 . ?
N1 C2 1.32(2) . ?
C2 H2 0.9300 . ?
C2 N2 1.32(2) . ?
N2 H2A 0.8600 . ?
C5 H5 0.9300 . ?
C5 N4 1.350(19) . ?
C5 C6 1.351(19) . ?
N4 H4 0.8600 . ?
N4 C4 1.351(19) . ?
C4 H4A 0.9300 . ?
C4 N3 1.350(19) . ?
N3 H3A 0.8600 . ?
N3 C6 1.351(19) . ?
C6 H6 0.9300 . ?

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 90.5(2) . . ?
Br1 Pb1 Br3 80.7(2) . 2_554 ?
Br1 Pb1 Br5 169.8(2) . . ?
Br1 Pb1 Br6 86.0(3) . 4_544 ?
Br2 Pb1 Br3 90.13(18) . 2_554 ?
Br2 Pb1 Br5 84.5(2) . . ?
Br2 Pb1 Br6 175.4(3) . 4_544 ?
Br3 Pb1 Br5 108.1(2) 2_554 . ?
Br4 Pb1 Br1 86.99(19) . . ?
Br4 Pb1 Br2 86.15(17) . . ?
Br4 Pb1 Br3 167.1(3) . 2_554 ?
Br4 Pb1 Br5 83.85(18) . . ?
Br4 Pb1 Br6 90.75(16) . 4_544 ?
Br6 Pb1 Br3 92.17(19) 4_544 2_554 ?
Br6 Pb1 Br5 98.5(3) 4_544 . ?
Br1 Pb2 Br4 105.30(18) 4_545 . ?
Br2 Pb2 Br1 168.23(18) . 4_545 ?
Br2 Pb2 Br4 83.49(17) . . ?
Br2 Pb2 Br5 85.9(2) . . ?
Br2 Pb2 Br6 86.1(2) . . ?
Br3 Pb2 Br1 84.2(2) . 4_545 ?
Br3 Pb2 Br2 86.47(18) . . ?
Br3 Pb2 Br4 169.35(16) . . ?
Br3 Pb2 Br5 92.8(2) . . ?
Br3 Pb2 Br6 81.8(2) . . ?
Br5 Pb2 Br1 87.4(3) . 4_545 ?
Br5 Pb2 Br4 82.98(19) . . ?
Br5 Pb2 Br6 170.59(17) . . ?
Br6 Pb2 Br1 99.6(3) . 4_545 ?
Br6 Pb2 Br4 101.0(2) . . ?
Pb1 Br1 Pb2 169.3(4) . 4_554 ?
Pb1 Br2 Pb2 78.78(19) . . ?
Pb2 Br3 Pb1 171.9(4) . 2 ?
Pb1 Br4 Pb2 78.68(11) . . ?
Pb2 Br5 Pb1 77.0(2) . . ?
Pb1 Br6 Pb2 150.4(3) 4 . ?
C1 C3 H3 126.0 . . ?
C1 C3 N2 108.0 . . ?
N2 C3 H3 126.0 . . ?
C3 C1 H1 126.0 . . ?
C3 C1 N1 108.0 . . ?
N1 C1 H1 126.0 . . ?
C1 N1 H1A 126.0 . . ?
C2 N1 C1 108.0 . . ?
C2 N1 H1A 126.0 . . ?
N1 C2 H2 126.0 . . ?
N1 C2 N2 108.0 . . ?
N2 C2 H2 126.0 . . ?
C3 N2 C2 108.0 . . ?
C3 N2 H2A 126.0 . . ?
C2 N2 H2A 126.0 . . ?
N4 C5 H5 126.0 . . ?
N4 C5 C6 108.0 . . ?
C6 C5 H5 126.0 . . ?
C5 N4 H4 126.0 . . ?
C5 N4 C4 108.0 . . ?
C4 N4 H4 126.0 . . ?
N4 C4 H4A 126.0 . . ?
N3 C4 N4 108.0 . . ?
N3 C4 H4A 126.0 . . ?
C4 N3 H3A 126.0 . . ?
C4 N3 C6 108.0 . . ?
C6 N3 H3A 126.0 . . ?
C5 C6 H6 126.0 . . ?
N3 C6 C5 108.0 . . ?
N3 C6 H6 126.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 C1 N1 C2 0.0 . . . . ?
C1 C3 N2 C2 0.0 . . . . ?
C1 N1 C2 N2 0.0 . . . . ?
N1 C2 N2 C3 0.0 . . . . ?
N2 C3 C1 N1 0.0 . . . . ?
C5 N4 C4 N3 0.0 . . . . ?
N4 C5 C6 N3 0.0 . . . . ?
N4 C4 N3 C6 0.0 . . . . ?
C4 N3 C6 C5 0.0 . . . . ?
C6 C5 N4 C4 0.0 . . . . ?

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

data_impbbr3_088gpa
_database_code_depnum_ccdc_archive 'CCDC 2473959'
loop_
_audit_author_name
_audit_author_address
'Kinga Roszak'
;Adam Mickiewicz University Poznan
Poland
;
_audit_update_record             
;
2025-07-18 deposited with the CCDC.	2026-03-26 downloaded from the CCDC.
;
_audit_creation_date             2024-07-31
# start Validation Reply Form
_vrf_PLAT027_impbbr3_088gpa      
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      15.00 Degree
RESPONSE: A full set of data was collected, however 
the very high angle data was poor and was omitted.
Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the 
X-ray radiation to the measured sample.
;
_vrf_PLAT029_impbbr3_088gpa      
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.449 Why?  
RESPONSE: The data come from high-pressure studies and are 
limited by the DAC opening angle.
;
_vrf_PLAT090_impbbr3_088gpa      
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       4.35 Note  
RESPONSE: The data/parameter ratio is affected by the access limits of the DAC.
;
_vrf_PLAT342_impbbr3_088gpa      
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............      0.095 Ang.  
RESPONSE: Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the X-ray 
radiation to the measured sample; poor quality of measurement
;
_vrf_PLAT911_impbbr3_088gpa      
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        198 Report
RESPONSE: These reflections were probably affected 
by unexpected deviations in their intensities for symmetry 
equivalent measurements and omitted during initial data reduction.
;
_vrf_PLAT987_impbbr3_088gpa      
;
PROBLEM: The Flack x is >> 0 -  Do a BASF/TWIN Refinement     Please Check 
RESPONSE: The structure was refined as an inversion twin.
;
# end Validation Reply Form
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br3 Pb, C3 H5 N2'
_chemical_formula_sum            'C3 H5 Br3 N2 Pb'
_chemical_formula_weight         516.01
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, z'

_cell_length_a                   13.8183(7)
_cell_length_b                   8.712(6)
_cell_length_c                   14.7579(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1776.6(11)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    2051
_cell_measurement_pressure       880000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.0130
_cell_measurement_theta_min      4.6460
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    32.411
_exptl_absorpt_correction_T_min  0.05205
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.858
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0931
_diffrn_reflns_av_unetI/netI     0.0765
_diffrn_reflns_Laue_measured_fraction_full 0.449
_diffrn_reflns_Laue_measured_fraction_max 0.329
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7528
_diffrn_reflns_point_group_measured_fraction_full 0.458
_diffrn_reflns_point_group_measured_fraction_max 0.331
_diffrn_reflns_theta_full        15.000
_diffrn_reflns_theta_max         26.739
_diffrn_reflns_theta_min         4.670
_diffrn_ambient_temperature      293(2)
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_detector_area_resol_mean 16.2413
_diffrn_measured_fraction_theta_full 0.449
_diffrn_measured_fraction_theta_max 0.329
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0086636556
_diffrn_orient_matrix_UB_12      -0.0801373341
_diffrn_orient_matrix_UB_13      -0.0008008583
_diffrn_orient_matrix_UB_21      0.0310986068
_diffrn_orient_matrix_UB_22      -0.0095901446
_diffrn_orient_matrix_UB_23      0.0378376199
_diffrn_orient_matrix_UB_31      -0.0399573378
_diffrn_orient_matrix_UB_32      0.0099529045
_diffrn_orient_matrix_UB_33      0.0296608826
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  19.75   0.75   35.00   0.00 -30.00   0.00    --    73
  2  φ    140.00 200.00   0.75   35.00   0.00 -30.00   0.00    --    80
  3  φ    160.00 217.00   0.75   35.00   0.00  30.00   0.00    --    76
  4  φ    -20.00  34.75   0.75   35.00   0.00  30.00   0.00    --    73
  5  ω    -24.00  24.00   0.75   35.00    --   30.00  39.46 -12.90   64
  6  ω    -24.00  24.00   0.75   35.00    --   30.00  39.46 167.10   64
  7  ω    -50.00  10.00   0.75   35.00    --  -30.00  39.46 167.10   80
  8  ω    -50.00  10.00   0.75   35.00    --  -30.00  39.46 -12.90   80
  9  ω    -64.00  -8.50   0.75   35.00    --  -30.00  81.40 -28.90   74
 10  ω    -64.00  -8.50   0.75   35.00    --  -30.00  81.40 151.10   74
 11  ω    -19.00   8.00   0.75   35.00    --   30.00  81.40 151.10   36
 12  ω    -19.00   8.00   0.75   35.00    --   30.00  81.40 -28.90   36
 13  ω    -43.00 -21.25   0.75   35.00    --   30.00 134.60 -56.90   29
 14  ω    -43.00 -21.25   0.75   35.00    --   30.00 134.60 123.10   29
 15  ω    -90.00 -36.00   0.75   35.00    --  -30.00 134.60 123.10   72
 16  ω    -90.00 -36.00   0.75   35.00    --  -30.00 134.60 -56.90   72
;
_diffrn_measurement_method       'ω and φ scans'
_reflns_Friedel_coverage         0.936
_reflns_Friedel_fraction_full    0.468
_reflns_Friedel_fraction_max     0.334
_reflns_number_gt                850
_reflns_number_total             1224
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXD  (Sheldrick, 2008)'
_refine_diff_density_max         0.794
_refine_diff_density_min         -0.634
_refine_diff_density_rms         0.167
_refine_ls_abs_structure_details 
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack   0.5
_refine_ls_extinction_coef       0.00071(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         1224
_refine_ls_number_restraints     165
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0405
_refine_ls_restrained_S_all      0.975
_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)+(0.0191P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0652
_refine_ls_wR_factor_ref         0.0767
_refine_special_details          
;
 Refined as a 2-component perfect inversion twin.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Rigid bond restraints
 N4, C4, N3, C6, C5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C3, N2, C2, N1, C1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Br1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Br5, Br3, Br6, Br2, Br4, Br1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C4 \\sim N3 \\sim C6 \\sim C5 \\sim N4: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
N2 \\sim C2 \\sim N1 \\sim C1 \\sim C3: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
C3 \\sim N2 \\sim C2 \\sim N1 \\sim C1: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Br1: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Br3 \\sim Br6 \\sim Br4 \\sim Br2 \\sim Br5 \\sim Br1: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(Br1) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(C4) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C5) \\sim
Ueq, Uanis(N4) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of
0.008
Uanis(C3) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C2) \\sim
Ueq, Uanis(N2) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of
0.008
Uanis(Pb2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(Br3) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(Br5) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4.a :
 C3(C1,N1,C2,N2), C6(C5,N4,C4,N3)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C1(H1), N1(H1A), C2(H2), N2(H2A), C6(H6), C5(H5), N4(H4), C4(H4A),
 N3(H3A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.1729(4) 0.0125(18) 0.36701(9) 0.030(4) Uani 1 1 d . . . . .
Pb2 Pb 0.1735(4) 0.0130(17) 0.62722(9) 0.0263(15) Uani 1 1 d . U . . .
Br1 Br 0.2305(10) 0.282(4) 0.2588(9) 0.043(5) Uani 1 1 d . U . . .
Br2 Br 0.0650(2) 0.2076(12) 0.4983(12) 0.045(6) Uani 1 1 d . . . . .
Br3 Br -0.0019(15) 0.002(5) 0.7443(12) 0.0346(14) Uani 1 1 d . U . . .
Br4 Br 0.33612(19) 0.0553(11) 0.4981(17) 0.040(6) Uani 1 1 d . . . . .
Br5 Br 0.1194(2) -0.2411(12) 0.4992(12) 0.0428(12) Uani 1 1 d . U . . .
Br6 Br 0.2342(9) 0.291(4) 0.7383(9) 0.039(9) Uani 1 1 d . . . . .
C3 C 0.369(2) 0.646(7) 0.446(4) 0.036(9) Uani 1 1 d G U . . .
H3 H 0.397387 0.721648 0.409936 0.043 Uiso 1 1 calc R U . . .
C1 C 0.379(2) 0.632(6) 0.534(4) 0.036(9) Uani 1 1 d G U . . .
H1 H 0.414509 0.696052 0.571930 0.044 Uiso 1 1 calc R U . . .
N1 N 0.329(3) 0.511(8) 0.560(3) 0.042(9) Uani 1 1 d G U . . .
H1A H 0.323312 0.477076 0.614771 0.051 Uiso 1 1 calc R U . . .
C2 C 0.2883(15) 0.450(6) 0.488(4) 0.047(9) Uani 1 1 d G U . . .
H2 H 0.248961 0.363055 0.486501 0.057 Uiso 1 1 calc R U . . .
N2 N 0.314(3) 0.533(8) 0.417(3) 0.043(9) Uani 1 1 d G U . . .
H2A H 0.296521 0.517100 0.361600 0.052 Uiso 1 1 calc R U . . .
C6 C 0.478(3) 0.068(10) 0.306(3) 0.040(9) Uani 1 1 d G U . . .
H6 H 0.463859 0.128234 0.356286 0.049 Uiso 1 1 calc R U . . .
C5 C 0.530(3) -0.053(10) 0.304(3) 0.040(9) Uani 1 1 d G U . . .
H5 H 0.561027 -0.097227 0.353975 0.047 Uiso 1 1 calc R U . . .
N4 N 0.533(2) -0.105(9) 0.218(4) 0.047(9) Uani 1 1 d G U . . .
H4 H 0.563564 -0.185923 0.200181 0.056 Uiso 1 1 calc R U . . .
C4 C 0.482(3) -0.018(9) 0.1657(17) 0.039(9) Uani 1 1 d G U . . .
H4A H 0.472137 -0.027367 0.103708 0.047 Uiso 1 1 calc R U . . .
N3 N 0.4487(19) 0.090(9) 0.220(3) 0.039(8) Uani 1 1 d G U . . .
H3A H 0.412308 0.164263 0.203272 0.046 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 2.95(3) . ?
Pb1 Br2 2.978(16) . ?
Pb1 Br3 2.981(18) 2_554 ?
Pb1 Br4 2.994(17) . ?
Pb1 Br5 3.038(19) . ?
Pb1 Br6 2.99(3) 3_544 ?
Pb2 Br1 3.10(3) 3_545 ?
Pb2 Br2 2.956(16) . ?
Pb2 Br3 2.978(18) . ?
Pb2 Br4 2.970(17) . ?
Pb2 Br5 3.005(18) . ?
Pb2 Br6 3.04(3) . ?
C3 H3 0.9300 . ?
C3 C1 1.32(2) . ?
C3 N2 1.32(2) . ?
C1 H1 0.9300 . ?
C1 N1 1.32(2) . ?
N1 H1A 0.8600 . ?
N1 C2 1.32(2) . ?
C2 H2 0.9300 . ?
C2 N2 1.32(2) . ?
N2 H2A 0.8600 . ?
C6 H6 0.9300 . ?
C6 C5 1.27(2) . ?
C6 N3 1.34(2) . ?
C5 H5 0.9300 . ?
C5 N4 1.36(2) . ?
N4 H4 0.8600 . ?
N4 C4 1.29(2) . ?
C4 H4A 0.9300 . ?
C4 N3 1.32(2) . ?
N3 H3A 0.8600 . ?

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 91.9(6) . . ?
Br1 Pb1 Br3 85.4(7) . 2_554 ?
Br1 Pb1 Br4 92.7(5) . . ?
Br1 Pb1 Br5 172.8(6) . . ?
Br1 Pb1 Br6 93.1(10) . 3_544 ?
Br2 Pb1 Br3 91.3(6) . 2_554 ?
Br2 Pb1 Br4 83.4(4) . . ?
Br2 Pb1 Br5 82.8(4) . . ?
Br2 Pb1 Br6 174.0(7) . 3_544 ?
Br3 Pb1 Br4 174.4(9) 2_554 . ?
Br3 Pb1 Br5 99.5(7) 2_554 . ?
Br3 Pb1 Br6 85.8(7) 2_554 3_544 ?
Br4 Pb1 Br5 81.9(4) . . ?
Br4 Pb1 Br6 99.6(4) . 3_544 ?
Br6 Pb1 Br5 92.5(7) 3_544 . ?
Br2 Pb2 Br1 173.7(7) . 3_545 ?
Br2 Pb2 Br3 88.8(6) . . ?
Br2 Pb2 Br4 84.2(4) . . ?
Br2 Pb2 Br5 83.8(4) . . ?
Br2 Pb2 Br6 91.7(7) . . ?
Br3 Pb2 Br1 88.0(7) . 3_545 ?
Br3 Pb2 Br5 98.0(7) . . ?
Br3 Pb2 Br6 86.4(7) . . ?
Br4 Pb2 Br1 99.1(4) . 3_545 ?
Br4 Pb2 Br3 172.8(8) . . ?
Br4 Pb2 Br5 82.9(4) . . ?
Br4 Pb2 Br6 92.2(4) . . ?
Br5 Pb2 Br1 91.3(7) . 3_545 ?
Br5 Pb2 Br6 173.6(6) . . ?
Br6 Pb2 Br1 93.5(10) . 3_545 ?
Pb1 Br1 Pb2 166.6(10) . 3_554 ?
Pb2 Br2 Pb1 80.6(2) . . ?
Pb2 Br3 Pb1 177.9(9) . 2 ?
Pb2 Br4 Pb1 80.17(8) . . ?
Pb2 Br5 Pb1 78.9(2) . . ?
Pb1 Br6 Pb2 166.4(10) 3 . ?
C1 C3 H3 126.0 . . ?
N2 C3 H3 126.0 . . ?
N2 C3 C1 108.0 . . ?
C3 C1 H1 126.0 . . ?
C3 C1 N1 108.0 . . ?
N1 C1 H1 126.0 . . ?
C1 N1 H1A 126.0 . . ?
C2 N1 C1 108.0 . . ?
C2 N1 H1A 126.0 . . ?
N1 C2 H2 126.0 . . ?
N1 C2 N2 108.0 . . ?
N2 C2 H2 126.0 . . ?
C3 N2 C2 108.0 . . ?
C3 N2 H2A 126.0 . . ?
C2 N2 H2A 126.0 . . ?
C5 C6 H6 127.2 . . ?
C5 C6 N3 105.7 . . ?
N3 C6 H6 127.2 . . ?
C6 C5 H5 125.9 . . ?
C6 C5 N4 108.2 . . ?
N4 C5 H5 125.9 . . ?
C5 N4 H4 124.9 . . ?
C4 N4 C5 110.2 . . ?
C4 N4 H4 124.9 . . ?
N4 C4 H4A 127.9 . . ?
N4 C4 N3 104.3 . . ?
N3 C4 H4A 127.9 . . ?
C6 N3 H3A 124.2 . . ?
C4 N3 C6 111.6 . . ?
C4 N3 H3A 124.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 C1 N1 C2 0.0 . . . . ?
C1 C3 N2 C2 0.0 . . . . ?
C1 N1 C2 N2 0.1 . . . . ?
N1 C2 N2 C3 0.0 . . . . ?
N2 C3 C1 N1 0.0 . . . . ?
C6 C5 N4 C4 0.0 . . . . ?
C5 C6 N3 C4 0.0 . . . . ?
C5 N4 C4 N3 0.0 . . . . ?
N4 C4 N3 C6 0.0 . . . . ?
N3 C6 C5 N4 0.0 . . . . ?

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

data_impbbr3_358gpa
_database_code_depnum_ccdc_archive 'CCDC 2473966'
loop_
_audit_author_name
_audit_author_address
'Kinga Roszak'
;Adam Mickiewicz University Poznan
Poland
;
_audit_update_record             
;
2025-07-18 deposited with the CCDC.	2026-03-26 downloaded from the CCDC.
;
_audit_creation_date             2024-08-01
# start Validation Reply Form
_vrf_PLAT029_impbbr3_358gpa      
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.372 Why?  
RESPONSE: A full set of data was collected, however 
the very high angle data was poor and was omitted.
Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the 
X-ray radiation to the measured sample.
;
_vrf_PLAT090_impbbr3_358gpa      
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       3.99 Note  
RESPONSE: The data/parameter ratio is affected by the access limits of the DAC.
;
_vrf_PLAT342_impbbr3_358gpa      
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............      0.115 Ang.  
RESPONSE: Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the X-ray 
radiation to the measured sample; poor quality of measurement
;
_vrf_PLAT911_impbbr3_358gpa      
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        185 Report
RESPONSE: These reflections were probably affected 
by unexpected deviations in their intensities for symmetry 
equivalent measurements and omitted during initial data reduction.
;
_vrf_PLAT973_impbbr3_358gpa      
;
PROBLEM: Check Calcd Positive Resid. Density on       Pb1       1.59 eA-3  
RESPONSE: The large residual densities all locate around on heavy
Pb atom
;
_vrf_PLAT987_impbbr3_358gpa      
;
PROBLEM: The Flack x is >> 0 -  Do a BASF/TWIN Refinement     Please Check 
RESPONSE: The structure was refined as an inversion twin.
;
# end Validation Reply Form
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br3 Pb, C3 H5 N2'
_chemical_formula_sum            'C3 H5 Br3 N2 Pb'
_chemical_formula_weight         516.01
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z+1/2'

_cell_length_a                   13.1813(17)
_cell_length_b                   8.300(8)
_cell_length_c                   14.3792(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1573.2(16)
_cell_formula_units_Z            8
_cell_measurement_pressure       3580000
_cell_measurement_reflns_used    1388
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.0870
_cell_measurement_theta_min      4.8000
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    36.603
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37721
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
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    4.357
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1670
_diffrn_reflns_av_unetI/netI     0.1454
_diffrn_reflns_Laue_measured_fraction_full 0.372
_diffrn_reflns_Laue_measured_fraction_max 0.337
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            5843
_diffrn_reflns_point_group_measured_fraction_full 0.377
_diffrn_reflns_point_group_measured_fraction_max 0.341
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.748
_diffrn_reflns_theta_min         4.862
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.2413
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.372
_diffrn_measured_fraction_theta_max 0.337
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  19.75   0.75   35.00   0.00 -30.00   0.00    --    73
  2  φ    140.00 200.00   0.75   35.00   0.00 -30.00   0.00    --    80
  3  φ    160.00 217.00   0.75   35.00   0.00  30.00   0.00    --    76
  4  φ    -20.00  34.75   0.75   35.00   0.00  30.00   0.00    --    73
  5  ω    -24.00  24.00   0.75   35.00    --   30.00  39.46 -12.90   64
  6  ω    -24.00  24.00   0.75   35.00    --   30.00  39.46 167.10   64
  7  ω    -50.00  10.00   0.75   35.00    --  -30.00  39.46 167.10   80
  8  ω    -50.00  10.00   0.75   35.00    --  -30.00  39.46 -12.90   80
  9  ω    -64.00  -8.50   0.75   35.00    --  -30.00  81.40 -28.90   74
 10  ω    -64.00  -8.50   0.75   35.00    --  -30.00  81.40 151.10   74
 11  ω    -19.00   8.00   0.75   35.00    --   30.00  81.40 151.10   36
 12  ω    -19.00   8.00   0.75   35.00    --   30.00  81.40 -28.90   36
 13  ω    -43.00 -21.25   0.75   35.00    --   30.00 134.60 -56.90   29
 14  ω    -43.00 -21.25   0.75   35.00    --   30.00 134.60 123.10   29
 15  ω    -90.00 -36.00   0.75   35.00    --  -30.00 134.60 123.10   72
 16  ω    -90.00 -36.00   0.75   35.00    --  -30.00 134.60 -56.90   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.942
_reflns_Friedel_fraction_full    0.382
_reflns_Friedel_fraction_max     0.345
_reflns_number_gt                606
_reflns_number_total             1074
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.131
_refine_diff_density_min         -1.312
_refine_diff_density_rms         0.287
_refine_ls_abs_structure_details 
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack   0.5
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     147
_refine_ls_number_reflns         1074
_refine_ls_number_restraints     193
_refine_ls_R_factor_all          0.1503
_refine_ls_R_factor_gt           0.0798
_refine_ls_restrained_S_all      0.994
_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)+(0.0568P)²+41.2781P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1487
_refine_ls_wR_factor_ref         0.1870
_refine_special_details          
;
 Refined as a 2-component perfect inversion twin.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 C3-C1
 1.36 with sigma of 0.02
 Br6-Br3 \\sim Br5-Br2 \\sim Br4-Br1
 with sigma of 0.02
3. Rigid bond restraints
 N2, C2, N1, C1, C3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C6, N3, C4, N4, C5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Br3, Br6, Br5, Br4, Br2, Br1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Pb1, Pb2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C3 \\sim C1 \\sim N1 \\sim C2 \\sim N2: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
N4 \\sim C4 \\sim N3 \\sim C6 \\sim C5: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Br5 \\sim Br2 \\sim Br4 \\sim Br1 \\sim Br6 \\sim Br3: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
Pb2 \\sim Pb1: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
Uanis(C3) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(N1) \\sim
Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of
0.008
Uanis(N3) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(N4) \\sim
Ueq, Uanis(C4) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of
0.008
Uanis(Br6) \\sim Ueq, Uanis(Br3) \\sim Ueq, Uanis(Br5) \\sim Ueq, Uanis(Br2)
\\sim Ueq, Uanis(Br4) \\sim Ueq, Uanis(Br1) \\sim Ueq: with sigma of 0.004 and
sigma for terminal atoms of 0.008
Uanis(Pb1) \\sim Ueq, Uanis(Pb2) \\sim Ueq: with sigma of 0.004 and sigma for
terminal atoms of 0.008
5.a :
 C1(N1,C2,N2,C3), N4(C4,N3,C6,C5)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), N1(H1A), C2(H2), N2(H2A), C3(H3), N4(H4), C4(H4A), N3(H3A), C6(H6),
 C5(H5)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.1665(3) -0.0109(11) 0.3677(3) 0.042(2) Uani 1 1 d . U . . .
Pb2 Pb 0.1868(3) 0.0039(11) 0.6263(2) 0.042(2) Uani 1 1 d . U . . .
Br1 Br 0.2275(8) 0.263(3) 0.2604(7) 0.050(4) Uani 1 1 d D U . . .
Br2 Br 0.0612(6) 0.202(2) 0.4994(8) 0.046(3) Uani 1 1 d D U . . .
Br3 Br 0.0078(8) -0.025(3) 0.7362(7) 0.043(4) Uani 1 1 d D U . . .
Br4 Br 0.3462(6) 0.040(3) 0.4760(6) 0.040(4) Uani 1 1 d D U . . .
Br5 Br 0.1245(7) -0.264(3) 0.5130(7) 0.047(3) Uani 1 1 d D U . . .
Br6 Br 0.2117(8) 0.312(4) 0.7341(7) 0.057(4) Uani 1 1 d D U . . .
C1 C 0.393(4) 0.644(12) 0.536(4) 0.039(12) Uani 1 1 d DG U . . .
H1 H 0.427070 0.721322 0.570737 0.047 Uiso 1 1 calc R U . . .
N1 N 0.331(4) 0.530(12) 0.571(4) 0.039(12) Uani 1 1 d G U . . .
H1A H 0.316902 0.516074 0.628507 0.047 Uiso 1 1 calc R U . . .
C2 C 0.297(4) 0.442(11) 0.500(5) 0.040(12) Uani 1 1 d G U . . .
H2 H 0.252612 0.355267 0.504067 0.048 Uiso 1 1 calc R U . . .
N2 N 0.337(4) 0.501(12) 0.422(4) 0.040(12) Uani 1 1 d G U . . .
H2A H 0.326004 0.465683 0.366303 0.048 Uiso 1 1 calc R U . . .
C3 C 0.396(4) 0.626(11) 0.444(4) 0.036(12) Uani 1 1 d DG U . . .
H3 H 0.432957 0.688993 0.402923 0.044 Uiso 1 1 calc R U . . .
N4 N 0.561(5) -0.121(15) 0.202(4) 0.053(14) Uani 1 1 d G U . . .
H4 H 0.586447 -0.204778 0.176212 0.063 Uiso 1 1 calc R U . . .
C4 C 0.499(5) 0.003(14) 0.156(5) 0.051(15) Uani 1 1 d G U . . .
H4A H 0.480656 0.005348 0.093893 0.061 Uiso 1 1 calc R U . . .
N3 N 0.471(5) 0.125(16) 0.227(4) 0.051(14) Uani 1 1 d G U . . .
H3A H 0.434541 0.209293 0.217359 0.061 Uiso 1 1 calc R U . . .
C6 C 0.515(5) 0.075(14) 0.316(5) 0.049(15) Uani 1 1 d G U . . .
H6 H 0.509044 0.129459 0.372561 0.059 Uiso 1 1 calc R U . . .
C5 C 0.571(5) -0.077(14) 0.301(5) 0.051(15) Uani 1 1 d G U . . .
H5 H 0.606141 -0.134826 0.346292 0.061 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 2.86(2) . ?
Pb1 Br2 2.941(16) . ?
Pb1 Br3 2.990(10) 2_554 ?
Pb1 Br4 2.866(10) . ?
Pb1 Br5 3.016(18) . ?
Pb1 Br6 2.904(18) 4_544 ?
Pb2 Br1 2.998(19) 4_545 ?
Pb2 Br2 2.966(16) . ?
Pb2 Br3 2.850(10) . ?
Pb2 Br4 3.029(10) . ?
Pb2 Br5 2.88(2) . ?
Pb2 Br6 3.01(3) . ?
C1 H1 0.9300 . ?
C1 N1 1.33(3) . ?
C1 C3 1.34(3) . ?
N1 H1A 0.8600 . ?
N1 C2 1.33(3) . ?
C2 H2 0.9300 . ?
C2 N2 1.33(3) . ?
N2 H2A 0.8600 . ?
N2 C3 1.33(3) . ?
C3 H3 0.9300 . ?
N4 H4 0.8600 . ?
N4 C4 1.47(7) . ?
N4 C5 1.47(7) . ?
C4 H4A 0.9300 . ?
C4 N3 1.47(7) . ?
N3 H3A 0.8600 . ?
N3 C6 1.47(7) . ?
C6 H6 0.9300 . ?
C6 C5 1.47(7) . ?
C5 H5 0.9300 . ?

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 90.1(5) . . ?
Br1 Pb1 Br3 78.2(5) . 2_554 ?
Br1 Pb1 Br4 86.8(4) . . ?
Br1 Pb1 Br5 168.2(4) . . ?
Br1 Pb1 Br6 83.7(6) . 4_544 ?
Br2 Pb1 Br3 89.1(4) . 2_554 ?
Br2 Pb1 Br5 83.5(4) . . ?
Br3 Pb1 Br5 111.5(4) 2_554 . ?
Br4 Pb1 Br2 87.2(4) . . ?
Br4 Pb1 Br3 164.5(7) . 2_554 ?
Br4 Pb1 Br5 83.0(4) . . ?
Br4 Pb1 Br6 88.7(4) . 4_544 ?
Br6 Pb1 Br2 172.8(7) 4_544 . ?
Br6 Pb1 Br3 93.3(4) 4_544 2_554 ?
Br6 Pb1 Br5 101.9(6) 4_544 . ?
Br1 Pb2 Br4 105.3(4) 4_545 . ?
Br1 Pb2 Br6 101.2(5) 4_545 . ?
Br2 Pb2 Br1 167.7(4) . 4_545 ?
Br2 Pb2 Br4 83.8(4) . . ?
Br2 Pb2 Br6 84.6(5) . . ?
Br3 Pb2 Br1 84.2(5) . 4_545 ?
Br3 Pb2 Br2 85.7(4) . . ?
Br3 Pb2 Br4 168.0(3) . . ?
Br3 Pb2 Br5 90.7(5) . . ?
Br3 Pb2 Br6 82.9(5) . . ?
Br5 Pb2 Br1 87.4(5) . 4_545 ?
Br5 Pb2 Br2 85.5(4) . . ?
Br5 Pb2 Br4 82.6(4) . . ?
Br5 Pb2 Br6 168.6(4) . . ?
Br6 Pb2 Br4 102.0(5) . . ?
Pb1 Br1 Pb2 169.1(8) . 4_554 ?
Pb1 Br2 Pb2 78.3(4) . . ?
Pb2 Br3 Pb1 168.0(9) . 2 ?
Pb1 Br4 Pb2 78.5(2) . . ?
Pb2 Br5 Pb1 78.5(5) . . ?
Pb1 Br6 Pb2 146.3(7) 4 . ?
N1 C1 H1 126.0 . . ?
N1 C1 C3 108.0 . . ?
C3 C1 H1 126.0 . . ?
C1 N1 H1A 126.0 . . ?
C1 N1 C2 108.0 . . ?
C2 N1 H1A 126.0 . . ?
N1 C2 H2 126.0 . . ?
N2 C2 N1 108.0 . . ?
N2 C2 H2 126.0 . . ?
C2 N2 H2A 126.0 . . ?
C3 N2 C2 108.0 . . ?
C3 N2 H2A 126.0 . . ?
C1 C3 H3 126.0 . . ?
N2 C3 C1 108.0 . . ?
N2 C3 H3 126.0 . . ?
C4 N4 H4 126.0 . . ?
C5 N4 H4 126.0 . . ?
C5 N4 C4 108.0 . . ?
N4 C4 H4A 126.0 . . ?
N3 C4 N4 108.0 . . ?
N3 C4 H4A 126.0 . . ?
C4 N3 H3A 126.0 . . ?
C6 N3 C4 108.0 . . ?
C6 N3 H3A 126.0 . . ?
N3 C6 H6 126.0 . . ?
N3 C6 C5 108.0 . . ?
C5 C6 H6 126.0 . . ?
N4 C5 C6 108.0 . . ?
N4 C5 H5 126.0 . . ?
C6 C5 H5 126.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N1 C2 N2 0.0 . . . . ?
N1 C1 C3 N2 0.0 . . . . ?
N1 C2 N2 C3 0.0 . . . . ?
C2 N2 C3 C1 0.0 . . . . ?
C3 C1 N1 C2 0.0 . . . . ?
N4 C4 N3 C6 0.0 . . . . ?
C4 N4 C5 C6 0.0 . . . . ?
C4 N3 C6 C5 0.0 . . . . ?
N3 C6 C5 N4 0.0 . . . . ?
C5 N4 C4 N3 0.0 . . . . ?

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

data_im3pbbr5_243gpa
_database_code_depnum_ccdc_archive 'CCDC 2473983'
loop_
_audit_author_name
_audit_author_address
'Kinga Roszak'
;Adam Mickiewicz University Poznan
Poland
;
_audit_update_record             
;
2025-07-18 deposited with the CCDC.	2026-03-26 downloaded from the CCDC.
;
_audit_creation_date             2025-04-14
# start Validation Reply Form
_vrf_PLAT029_im3pbbr5_243gpa     
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.240 Why?  
RESPONSE: The data come from high-pressure studies and are 
limited by the DAC opening angle.
;
_vrf_PLAT090_im3pbbr5_243gpa     
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       2.38 Note  
RESPONSE:  The data/parameter ratio is affected by the access limits of the DAC.
;
_vrf_PLAT342_im3pbbr5_243gpa     
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.12333 Ang.  
RESPONSE: Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the X-ray 
radiation to the measured sample
;
_vrf_PLAT910_im3pbbr5_243gpa     
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         12 Note  
RESPONSE: These reflections were probably affected 
by unexpected deviations in their intensities for symmetry 
equivalent measurements and omitted during initial data reduction.
;
_vrf_PLAT911_im3pbbr5_243gpa     
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        863 Report
RESPONSE: These reflections were probably affected 
by unexpected deviations in their intensities for symmetry 
equivalent measurements and omitted during initial data reduction.
;
_vrf_PLAT915_im3pbbr5_243gpa     
;
PROBLEM: No Flack x Check Done: Low Friedel Pair Coverage         21 %     
RESPONSE: Because the Friedel Pair Coverage was low the absolute configuration was
assigned using the known absolute configuration of the molecules
;
_vrf_PLAT987_im3pbbr5_243gpa     
;
PROBLEM: The Flack x is >> 0 -  Do a BASF/TWIN Refinement     Please Check 
RESPONSE: As indicated by the Flack
parameter, the structures were refined as twins. 
All refinements converged to the racemic-twin compounds.
;
# end Validation Reply Form
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br5 Pb, 3(C3 H5 N2)'
_chemical_formula_sum            'C9 H15 Br5 N6 Pb'
_chemical_formula_weight         814.01
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   5.8912(5)
_cell_length_b                   9.0889(19)
_cell_length_c                   8.999(3)
_cell_angle_alpha                65.73(3)
_cell_angle_beta                 83.808(16)
_cell_angle_gamma                86.707(14)
_cell_volume                     436.6(2)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    1132
_cell_measurement_pressure       2430000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.3030
_cell_measurement_theta_min      4.6120
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    21.100
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.03565
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.096
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             368
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0488
_diffrn_reflns_av_unetI/netI     0.0578
_diffrn_reflns_Laue_measured_fraction_full 0.240
_diffrn_reflns_Laue_measured_fraction_max 0.214
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            2206
_diffrn_reflns_point_group_measured_fraction_full 0.240
_diffrn_reflns_point_group_measured_fraction_max 0.214
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.659
_diffrn_reflns_theta_min         4.609
_diffrn_ambient_temperature      293(2)
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_detector_area_resol_mean 16.2413
_diffrn_measured_fraction_theta_full 0.240
_diffrn_measured_fraction_theta_max 0.214
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0142791871
_diffrn_orient_matrix_UB_12      -0.0446765341
_diffrn_orient_matrix_UB_13      0.0860675690
_diffrn_orient_matrix_UB_21      -0.1195882036
_diffrn_orient_matrix_UB_22      0.0142685089
_diffrn_orient_matrix_UB_23      -0.0008993776
_diffrn_orient_matrix_UB_31      -0.0128235239
_diffrn_orient_matrix_UB_32      -0.0716276769
_diffrn_orient_matrix_UB_33      -0.0115205783
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  19.75   0.75   35.00   0.00 -30.00   0.00    --    73
  2  φ    140.00 200.00   0.75   35.00   0.00 -30.00   0.00    --    80
  3  φ    160.00 217.00   0.75   35.00   0.00  30.00   0.00    --    76
  4  φ    -20.00  34.75   0.75   35.00   0.00  30.00   0.00    --    73
  5  ω    -24.00  24.00   0.75   35.00    --   30.00  39.46 -12.90   64
  6  ω    -24.00  24.00   0.75   35.00    --   30.00  39.46 167.10   64
  7  ω    -50.00  10.00   0.75   35.00    --  -30.00  39.46 167.10   80
  8  ω    -50.00  10.00   0.75   35.00    --  -30.00  39.46 -12.90   80
  9  ω    -64.00  -8.50   0.75   35.00    --  -30.00  81.40 -28.90   74
 10  ω    -64.00  -8.50   0.75   35.00    --  -30.00  81.40 151.10   74
 11  ω    -19.00   8.00   0.75   35.00    --   30.00  81.40 151.10   36
 12  ω    -19.00   8.00   0.75   35.00    --   30.00  81.40 -28.90   36
 13  ω    -43.00 -21.25   0.75   35.00    --   30.00 134.60 -56.90   29
 14  ω    -43.00 -21.25   0.75   35.00    --   30.00 134.60 123.10   29
 15  ω    -90.00 -36.00   0.75   35.00    --  -30.00 134.60 123.10   72
 16  ω    -90.00 -36.00   0.75   35.00    --  -30.00 134.60 -56.90   72
;
_diffrn_measurement_method       'ω and φ scans'
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.240
_reflns_Friedel_fraction_max     0.214
_reflns_number_gt                688
_reflns_number_total             777
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXD  (Sheldrick, 2008)'
_refine_diff_density_max         0.458
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.120
_refine_ls_abs_structure_details 
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack   0.5
_refine_ls_extinction_coef       0.009(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         777
_refine_ls_number_restraints     245
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0438
_refine_ls_restrained_S_all      1.003
_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)+(0.0409P)²+6.1356P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0954
_refine_ls_wR_factor_ref         0.0995
_refine_special_details          
;
 Refined as a 2-component perfect inversion twin.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 C5-C4
 1.28 with sigma of 0.02
 C9-C8
 2.1 with sigma of 0.02
3. Rigid bond restraints
 N3, C6, N4, C5, C4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N2, C1, N1, C2, C3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N6, C9, N5, C8, C7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Br3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Br5, Br2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C5 \\sim N4 \\sim N3 \\sim C6 \\sim C4: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
C3 \\sim C2 \\sim N1 \\sim C1 \\sim N2: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
C9 \\sim N5 \\sim C8 \\sim C7 \\sim N6: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Br3: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Br2 \\sim Br5: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
Uanis(C9) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C7) \\sim
Ueq, Uanis(N6) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of
0.008
Uanis(C5) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C6) \\sim
Ueq, Uanis(N4) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of
0.008
Uanis(C3) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C1) \\sim
Ueq, Uanis(N2) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of
0.008
Uanis(Br3) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(Br5) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(Br2) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(Br1) \\sim Ueq, Uanis(Br4) \\sim Ueq: with sigma of 0.004 and sigma for
terminal atoms of 0.008
5.a :
 C3(N2,C1,N1,C2), N3(C6,N4,C5,C4), C9(N5,C8,C7,N6)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), N2(H2), C1(H1), N1(H1A), C2(H2A), N3(H3A), C6(H6), N4(H4), C5(H5),
 C4(H4A), C9(H9), N5(H5A), C8(H8), C7(H7), N6(H6A)
;
_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 1.4996(5) 0.5080(7) -0.0147(11) 0.044(5) Uani 1 1 d . . . . .
Br1 Br 1.484(2) 0.168(3) 0.250(5) 0.054(7) Uani 1 1 d . U . . .
Br2 Br 1.5225(19) 0.374(2) -0.266(5) 0.039(6) Uani 1 1 d . U . . .
Br3 Br 1.003(2) 0.527(3) -0.018(5) 0.041(4) Uani 1 1 d . U . . .
Br4 Br 1.464(2) 0.629(3) 0.249(5) 0.048(6) Uani 1 1 d . U . . .
Br5 Br 1.5108(17) 0.839(2) -0.257(4) 0.032(6) Uani 1 1 d . U . . .
C3 C 0.906(9) -0.103(10) 1.001(19) 0.037(12) Uani 1 1 d G U . . .
H3 H 0.832652 -0.195254 1.012874 0.045 Uiso 1 1 calc R U . . .
N2 N 1.126(8) -0.091(9) 1.015(18) 0.042(11) Uani 1 1 d G U . . .
H2 H 1.225383 -0.168684 1.037182 0.050 Uiso 1 1 calc R U . . .
C1 C 1.168(8) 0.060(10) 0.990(19) 0.044(12) Uani 1 1 d G U . . .
H1 H 1.307785 0.100478 0.993056 0.052 Uiso 1 1 calc R U . . .
N1 N 0.973(10) 0.142(9) 0.960(18) 0.041(11) Uani 1 1 d G U . . .
H1A H 0.953896 0.242520 0.940267 0.049 Uiso 1 1 calc R U . . .
C2 C 0.812(7) 0.041(10) 0.967(19) 0.044(12) Uani 1 1 d G U . . .
H2A H 0.658953 0.068235 0.950795 0.053 Uiso 1 1 calc R U . . .
N3 N 1.155(8) 0.319(9) 0.516(17) 0.046(11) Uani 1 1 d G U . . .
H3A H 1.267712 0.373858 0.518648 0.055 Uiso 1 1 calc R U . . .
C6 C 0.988(10) 0.375(9) 0.427(16) 0.043(11) Uani 1 1 d G U . . .
H6 H 0.966528 0.481423 0.355312 0.052 Uiso 1 1 calc R U . . .
N4 N 0.853(8) 0.257(10) 0.456(17) 0.045(11) Uani 1 1 d G U . . .
H4 H 0.728956 0.263640 0.411424 0.054 Uiso 1 1 calc R U . . .
C5 C 0.938(9) 0.129(9) 0.562(17) 0.038(12) Uani 1 1 d DG U . . .
H5 H 0.875888 0.026352 0.604180 0.046 Uiso 1 1 calc R U . . .
C4 C 1.124(9) 0.167(9) 0.598(16) 0.045(12) Uani 1 1 d DG U . . .
H4A H 1.220648 0.097002 0.672589 0.053 Uiso 1 1 calc R U . . .
C9 C 1.093(7) -0.302(9) 0.548(14) 0.040(10) Uani 1 1 d DG U . . .
H9 H 1.176672 -0.381346 0.625252 0.048 Uiso 1 1 calc R U . . .
N5 N 1.149(7) -0.153(9) 0.468(16) 0.033(9) Uani 1 1 d G U . . .
H5A H 1.269717 -0.108519 0.475564 0.039 Uiso 1 1 calc R U . . .
C8 C 0.989(9) -0.082(8) 0.373(15) 0.037(10) Uani 1 1 d DG U . . .
H8 H 0.985651 0.026497 0.301116 0.044 Uiso 1 1 calc R U . . .
C7 C 0.834(8) -0.188(9) 0.395(15) 0.036(11) Uani 1 1 d G U . . .
H7 H 0.701694 -0.168335 0.341749 0.044 Uiso 1 1 calc R U . . .
N6 N 0.898(8) -0.324(8) 0.503(15) 0.036(10) Uani 1 1 d G U . . .
H6A H 0.825883 -0.413419 0.539480 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 Br1 3.03(4) . ?
Pb1 Br2 2.96(3) . ?
Pb1 Br3 2.921(12) . ?
Pb1 Br3 2.979(12) 1_655 ?
Pb1 Br4 2.99(3) . ?
Pb1 Br5 2.90(3) . ?
C3 H3 0.9300 . ?
C3 N2 1.33(3) . ?
C3 C2 1.32(3) . ?
N2 H2 0.8600 . ?
N2 C1 1.33(3) . ?
C1 H1 0.9300 . ?
C1 N1 1.32(3) . ?
N1 H1A 0.8600 . ?
N1 C2 1.34(3) . ?
C2 H2A 0.9300 . ?
N3 H3A 0.8600 . ?
N3 C6 1.28(3) . ?
N3 C4 1.28(3) . ?
C6 H6 0.9300 . ?
C6 N4 1.29(3) . ?
N4 H4 0.8600 . ?
N4 C5 1.28(3) . ?
C5 H5 0.9300 . ?
C5 C4 1.29(3) . ?
C4 H4A 0.9300 . ?
C9 H9 0.9300 . ?
C9 N5 1.29(2) . ?
C9 N6 1.31(2) . ?
N5 H5A 0.8600 . ?
N5 C8 1.30(2) . ?
C8 H8 0.9300 . ?
C8 C7 1.31(2) . ?
C7 H7 0.9300 . ?
C7 N6 1.29(2) . ?
N6 H6A 0.8600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br2 Pb1 Br1 89.5(10) . . ?
Br2 Pb1 Br3 95.3(6) . 1_655 ?
Br2 Pb1 Br4 177.3(11) . . ?
Br3 Pb1 Br1 92.8(7) 1_655 . ?
Br3 Pb1 Br1 92.3(7) . . ?
Br3 Pb1 Br2 88.4(6) . . ?
Br3 Pb1 Br3 173.7(6) . 1_655 ?
Br3 Pb1 Br4 90.3(6) . . ?
Br3 Pb1 Br4 86.2(7) 1_655 . ?
Br4 Pb1 Br1 88.2(7) . . ?
Br5 Pb1 Br1 177.4(10) . . ?
Br5 Pb1 Br2 93.1(7) . . ?
Br5 Pb1 Br3 87.4(7) . . ?
Br5 Pb1 Br3 87.3(7) . 1_655 ?
Br5 Pb1 Br4 89.2(9) . . ?
Pb1 Br3 Pb1 173.7(6) . 1_455 ?
N2 C3 H3 126.3 . . ?
C2 C3 H3 126.3 . . ?
C2 C3 N2 107.4 . . ?
C3 N2 H2 125.6 . . ?
C1 N2 C3 108.8 . . ?
C1 N2 H2 125.6 . . ?
N2 C1 H1 126.3 . . ?
N1 C1 N2 107.36(6) . . ?
N1 C1 H1 126.3 . . ?
C1 N1 H1A 125.9 . . ?
C1 N1 C2 108.3 . . ?
C2 N1 H1A 125.9 . . ?
C3 C2 N1 108.2 . . ?
C3 C2 H2A 125.9 . . ?
N1 C2 H2A 125.9 . . ?
C6 N3 H3A 126.3 . . ?
C6 N3 C4 107.5 . . ?
C4 N3 H3A 126.3 . . ?
N3 C6 H6 125.8 . . ?
N3 C6 N4 108.4 . . ?
N4 C6 H6 125.8 . . ?
C6 N4 H4 126.0 . . ?
C5 N4 C6 108.0 . . ?
C5 N4 H4 126.0 . . ?
N4 C5 H5 126.1 . . ?
N4 C5 C4 107.7 . . ?
C4 C5 H5 126.1 . . ?
N3 C4 C5 108.5 . . ?
N3 C4 H4A 125.8 . . ?
C5 C4 H4A 125.8 . . ?
N5 C9 H9 125.7 . . ?
N5 C9 N6 108.6 . . ?
N6 C9 H9 125.7 . . ?
C9 N5 H5A 126.4 . . ?
C9 N5 C8 107.2 . . ?
C8 N5 H5A 126.4 . . ?
N5 C8 H8 125.6 . . ?
N5 C8 C7 108.7 . . ?
C7 C8 H8 125.6 . . ?
C8 C7 H7 126.2 . . ?
N6 C7 C8 107.7 . . ?
N6 C7 H7 126.2 . . ?
C9 N6 H6A 126.1 . . ?
C7 N6 C9 107.8 . . ?
C7 N6 H6A 126.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 N2 C1 N1 0.0 . . . . ?
N2 C3 C2 N1 0.0 . . . . ?
N2 C1 N1 C2 0.0 . . . . ?
C1 N1 C2 C3 0.0 . . . . ?
C2 C3 N2 C1 0.0 . . . . ?
N3 C6 N4 C5 0.0 . . . . ?
C6 N3 C4 C5 0.0 . . . . ?
C6 N4 C5 C4 0.0 . . . . ?
N4 C5 C4 N3 0.0 . . . . ?
C4 N3 C6 N4 0.0 . . . . ?
C9 N5 C8 C7 0.0 . . . . ?
N5 C9 N6 C7 0.0 . . . . ?
N5 C8 C7 N6 0.0 . . . . ?
C8 C7 N6 C9 0.0 . . . . ?
N6 C9 N5 C8 0.0 . . . . ?

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

data_im3pbbr5_204gpa
_database_code_depnum_ccdc_archive 'CCDC 2473982'
loop_
_audit_author_name
_audit_author_address
'Kinga Roszak'
;Adam Mickiewicz University Poznan
Poland
;
_audit_update_record             
;
2025-07-18 deposited with the CCDC.	2026-03-26 downloaded from the CCDC.
;
_audit_creation_date             2024-08-27
# start Validation Reply Form
_vrf_PLAT027_im3pbbr5_204gpa     
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      17.50 Degree
RESPONSE: A full set of data was collected, however 
the very high angle data was poor and was omitted.
Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the 
X-ray radiation to the measured sample.
;
_vrf_PLAT029_im3pbbr5_204gpa     
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.320 Why?  
RESPONSE: The data come from high-pressure studies and are 
limited by the DAC opening angle.
;
_vrf_PLAT090_im3pbbr5_204gpa     
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       2.44 Note  
RESPONSE:  The data/parameter ratio is affected by the access limits of the DAC.
;
_vrf_PLAT342_im3pbbr5_204gpa     
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............        0.1 Ang.  
RESPONSE: Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the X-ray 
radiation to the measured sample
;
_vrf_PLAT910_im3pbbr5_204gpa     
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         12 Note  
RESPONSE: These reflections were probably affected 
by unexpected deviations in their intensities for symmetry 
equivalent measurements and omitted during initial data reduction.
;
_vrf_PLAT911_im3pbbr5_204gpa     
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        861 Report
RESPONSE: These reflections were probably affected 
by unexpected deviations in their intensities for symmetry 
equivalent measurements and omitted during initial data reduction.
;
_vrf_PLAT915_im3pbbr5_204gpa     
;
PROBLEM: No Flack x Check Done: Low Friedel Pair Coverage         20 %     
RESPONSE: Because the Friedel Pair Coverage was low the absolute configuration was
assigned using the known absolute configuration of the molecules
;
_vrf_PLAT987_im3pbbr5_204gpa     
;
PROBLEM: The Flack x is >> 0 -  Do a BASF/TWIN Refinement     Please Check 
RESPONSE: As indicated by the Flack
parameter, the structures were refined as twins. 
All refinements converged to the racemic-twin compounds.
;
# end Validation Reply Form

_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br5 Pb, 3(C3 H5 N2)'
_chemical_formula_sum            'C9 H15 Br5 N6 Pb'
_chemical_formula_weight         813.97
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         C9H15Br5N6Pb
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   5.9165(5)
_cell_length_b                   9.1040(18)
_cell_length_c                   9.066(3)
_cell_angle_alpha                65.96(3)
_cell_angle_beta                 84.090(16)
_cell_angle_gamma                86.978(14)
_cell_volume                     443.6(2)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    1100
_cell_measurement_pressure       2040000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.2810
_cell_measurement_theta_min      4.5770
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    20.771
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.04076
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.89a (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_density_diffrn    3.047
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             368
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0506
_diffrn_reflns_av_unetI/netI     0.0644
_diffrn_reflns_Laue_measured_fraction_full 0.320
_diffrn_reflns_Laue_measured_fraction_max 0.216
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            2214
_diffrn_reflns_point_group_measured_fraction_full 0.320
_diffrn_reflns_point_group_measured_fraction_max 0.216
_diffrn_reflns_theta_full        17.500
_diffrn_reflns_theta_max         26.650
_diffrn_reflns_theta_min         4.576
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2413
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.320
_diffrn_measured_fraction_theta_max 0.216
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  19.75   0.75   35.00   0.00 -30.00   0.00    --    73
  2  φ    140.00 200.00   0.75   35.00   0.00 -30.00   0.00    --    80
  3  φ    160.00 217.00   0.75   35.00   0.00  30.00   0.00    --    76
  4  φ    -20.00  34.75   0.75   35.00   0.00  30.00   0.00    --    73
  5  ω    -24.00  24.00   0.75   35.00    --   30.00  39.46 -12.90   64
  6  ω    -24.00  24.00   0.75   35.00    --   30.00  39.46 167.10   64
  7  ω    -50.00  10.00   0.75   35.00    --  -30.00  39.46 167.10   80
  8  ω    -50.00  10.00   0.75   35.00    --  -30.00  39.46 -12.90   80
  9  ω    -64.00  -8.50   0.75   35.00    --  -30.00  81.40 -28.90   74
 10  ω    -64.00  -8.50   0.75   35.00    --  -30.00  81.40 151.10   74
 11  ω    -19.00   8.00   0.75   35.00    --   30.00  81.40 151.10   36
 12  ω    -19.00   8.00   0.75   35.00    --   30.00  81.40 -28.90   36
 13  ω    -43.00 -21.25   0.75   35.00    --   30.00 134.60 -56.90   29
 14  ω    -43.00 -21.25   0.75   35.00    --   30.00 134.60 123.10   29
 15  ω    -90.00 -36.00   0.75   35.00    --  -30.00 134.60 123.10   72
 16  ω    -90.00 -36.00   0.75   35.00    --  -30.00 134.60 -56.90   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_axis[1]    matrixX
_diffrn_orient_matrix_axis[2]    matrixY
_diffrn_orient_matrix_axis[3]    matrixZ
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0139499633
_diffrn_orient_matrix_UB_12      -0.0442342333
_diffrn_orient_matrix_UB_13      0.0852519217
_diffrn_orient_matrix_UB_21      -0.1190230693
_diffrn_orient_matrix_UB_22      0.0139934640
_diffrn_orient_matrix_UB_23      -0.0009720139
_diffrn_orient_matrix_UB_31      -0.0129391272
_diffrn_orient_matrix_UB_32      -0.0715989247
_diffrn_orient_matrix_UB_33      -0.0113844451
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.320
_reflns_Friedel_fraction_max     0.216
_reflns_number_gt                650
_reflns_number_total             785
_reflns_odcompleteness_completeness 22.24
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXD  (Sheldrick, 2008)'
_refine_diff_density_max         0.376
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.101
_refine_ls_abs_structure_details 
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack   0.5
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         785
_refine_ls_number_restraints     225
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0369
_refine_ls_restrained_S_all      0.908
_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)+(0.0407P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0760
_refine_ls_wR_factor_ref         0.0811
_refine_special_details          
;
 Refined as a 2-component perfect inversion twin.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Rigid bond restraints
 C1, N1, C2, C3, N2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N3, C4, C5, N4, C6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C9, N5, C8, C7, N6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Br4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Br1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
N2 \\sim C1 \\sim N1 \\sim C3 \\sim C2: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
C4 \\sim C5 \\sim N4 \\sim C6 \\sim N3: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
N6 \\sim C7 \\sim C8 \\sim N5 \\sim C9: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Br4: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Br1: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(C1) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim
Ueq, Uanis(N2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(N3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(N4) \\sim
Ueq, Uanis(C6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(N6) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(C8) \\sim
Ueq, Uanis(C7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(Br4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Br1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a :
 C3(N2,C1,N1,C2), N3(C6,N4,C5,C4), C9(N5,C8,C7,N6)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), N2(H2), C1(H1), N1(H1A), C2(H2A), N3(H3A), C6(H6), N4(H4), C5(H5),
 C4(H4A), C9(H9), N5(H5A), C8(H8), C7(H7), N6(H6A)
;
_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 1.4905(12) 0.5006(18) 0.000(3) 0.041(4) Uani 1 1 d . . . . .
Br1 Br 1.4777(17) 0.162(2) 0.259(5) 0.043(13) Uani 1 1 d . U . . .
Br2 Br 1.5189(16) 0.375(3) -0.261(5) 0.062(19) Uani 1 1 d . . . . .
Br3 Br 0.987(3) 0.501(5) 0.009(10) 0.046(13) Uani 1 1 d . . . . .
Br4 Br 1.4629(17) 0.627(2) 0.255(5) 0.043(12) Uani 1 1 d . U . . .
Br5 Br 1.5028(17) 0.832(3) -0.245(5) 0.087(19) Uani 1 1 d . . . . .
C3 C 1.008(11) -0.118(8) 0.995(16) 0.035(13) Uani 1 1 d G U . . .
H3 H 1.017883 -0.221394 0.997010 0.042 Uiso 1 1 calc R U . . .
N2 N 1.170(6) -0.042(9) 1.020(15) 0.039(11) Uani 1 1 d G U . . .
H2 H 1.305605 -0.078340 1.042091 0.047 Uiso 1 1 calc R U . . .
C1 C 1.093(9) 0.100(8) 1.007(15) 0.035(12) Uani 1 1 d G U . . .
H1 H 1.173452 0.178618 1.019673 0.042 Uiso 1 1 calc R U . . .
N1 N 0.882(8) 0.111(8) 0.974(15) 0.034(11) Uani 1 1 d G U . . .
H1A H 0.793038 0.192639 0.959093 0.041 Uiso 1 1 calc R U . . .
C2 C 0.830(8) -0.024(10) 0.966(17) 0.043(13) Uani 1 1 d G U . . .
H2A H 0.689690 -0.047789 0.943881 0.052 Uiso 1 1 calc R U . . .
N3 N 1.149(8) 0.326(9) 0.521(14) 0.048(13) Uani 1 1 d G U . . .
H3A H 1.261218 0.384124 0.517778 0.058 Uiso 1 1 calc R U . . .
C6 C 0.983(9) 0.373(8) 0.426(15) 0.044(12) Uani 1 1 d G U . . .
H6 H 0.964558 0.474089 0.344471 0.053 Uiso 1 1 calc R U . . .
N4 N 0.845(8) 0.250(8) 0.468(15) 0.040(12) Uani 1 1 d G U . . .
H4 H 0.723101 0.250491 0.424092 0.048 Uiso 1 1 calc R U . . .
C5 C 0.927(8) 0.128(8) 0.588(14) 0.046(14) Uani 1 1 d G U . . .
H5 H 0.863426 0.026883 0.640764 0.055 Uiso 1 1 calc R U . . .
C4 C 1.115(8) 0.175(8) 0.621(13) 0.042(13) Uani 1 1 d G U . . .
H4A H 1.207792 0.112441 0.700582 0.050 Uiso 1 1 calc R U . . .
C9 C 1.087(7) -0.305(8) 0.551(13) 0.049(13) Uani 1 1 d G U . . .
H9 H 1.174783 -0.385110 0.622621 0.059 Uiso 1 1 calc R U . . .
N5 N 1.146(7) -0.153(8) 0.468(14) 0.034(11) Uani 1 1 d G U . . .
H5A H 1.270980 -0.110889 0.470984 0.040 Uiso 1 1 calc R U . . .
C8 C 0.976(8) -0.078(8) 0.381(14) 0.044(12) Uani 1 1 d G U . . .
H8 H 0.972236 0.030148 0.310975 0.053 Uiso 1 1 calc R U . . .
C7 C 0.813(9) -0.184(8) 0.409(14) 0.041(13) Uani 1 1 d G U . . .
H7 H 0.675205 -0.162251 0.363200 0.049 Uiso 1 1 calc R U . . .
N6 N 0.882(8) -0.324(7) 0.515(13) 0.040(12) Uani 1 1 d G U . . .
H6A H 0.806675 -0.411883 0.552993 0.048 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br1 3.02(4) . ?
Pb1 Br2 3.01(4) . ?
Pb1 Br3 2.948(17) 1_655 ?
Pb1 Br3 2.971(17) . ?
Pb1 Br4 2.96(3) . ?
Pb1 Br5 2.93(4) . ?
C3 H3 0.9300 . ?
C3 N2 1.31(2) . ?
C3 C2 1.30(2) . ?
N2 H2 0.8600 . ?
N2 C1 1.31(2) . ?
C1 H1 0.9300 . ?
C1 N1 1.30(2) . ?
N1 H1A 0.8600 . ?
N1 C2 1.31(2) . ?
C2 H2A 0.9300 . ?
N3 H3A 0.8600 . ?
N3 C6 1.31(4) . ?
N3 C4 1.31(4) . ?
C6 H6 0.9300 . ?
C6 N4 1.32(4) . ?
N4 H4 0.8600 . ?
N4 C5 1.31(4) . ?
C5 H5 0.9300 . ?
C5 C4 1.31(4) . ?
C4 H4A 0.9300 . ?
C9 H9 0.9300 . ?
C9 N5 1.32(4) . ?
C9 N6 1.33(4) . ?
N5 H5A 0.8600 . ?
N5 C8 1.32(4) . ?
C8 H8 0.9300 . ?
C8 C7 1.33(4) . ?
C7 H7 0.9300 . ?
C7 N6 1.32(4) . ?
N6 H6A 0.8600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br2 Pb1 Br1 90.9(10) . . ?
Br3 Pb1 Br1 89.5(11) . . ?
Br3 Pb1 Br1 89.4(12) 1_655 . ?
Br3 Pb1 Br2 88.8(10) . . ?
Br3 Pb1 Br2 94.0(10) 1_655 . ?
Br3 Pb1 Br3 177(2) 1_655 . ?
Br3 Pb1 Br4 86.0(10) 1_655 . ?
Br4 Pb1 Br1 89.7(10) . . ?
Br4 Pb1 Br2 179.4(16) . . ?
Br4 Pb1 Br3 91.2(9) . . ?
Br5 Pb1 Br1 178.6(13) . . ?
Br5 Pb1 Br2 90.5(10) . . ?
Br5 Pb1 Br3 90.6(12) . . ?
Br5 Pb1 Br3 90.5(11) . 1_655 ?
Br5 Pb1 Br4 88.9(11) . . ?
Pb1 Br3 Pb1 177(2) 1_455 . ?
N2 C3 H3 126.2 . . ?
C2 C3 H3 126.2 . . ?
C2 C3 N2 107.6 . . ?
C3 N2 H2 125.8 . . ?
C3 N2 C1 108.5 . . ?
C1 N2 H2 125.8 . . ?
N2 C1 H1 126.2 . . ?
N1 C1 N2 107.7 . . ?
N1 C1 H1 126.2 . . ?
C1 N1 H1A 126.0 . . ?
C1 N1 C2 108.1 . . ?
C2 N1 H1A 126.0 . . ?
C3 C2 N1 108.2 . . ?
C3 C2 H2A 125.9 . . ?
N1 C2 H2A 125.9 . . ?
C6 N3 H3A 126.1 . . ?
C6 N3 C4 107.8 . . ?
C4 N3 H3A 126.1 . . ?
N3 C6 H6 126.0 . . ?
N3 C6 N4 108.1 . . ?
N4 C6 H6 126.0 . . ?
C6 N4 H4 126.0 . . ?
C5 N4 C6 108.1 . . ?
C5 N4 H4 126.0 . . ?
N4 C5 H5 126.1 . . ?
N4 C5 C4 107.8 . . ?
C4 C5 H5 126.1 . . ?
N3 C4 H4A 125.9 . . ?
C5 C4 N3 108.2 . . ?
C5 C4 H4A 125.9 . . ?
N5 C9 H9 125.8 . . ?
N5 C9 N6 108.3 . . ?
N6 C9 H9 125.8 . . ?
C9 N5 H5A 126.2 . . ?
C9 N5 C8 107.5 . . ?
C8 N5 H5A 126.2 . . ?
N5 C8 H8 125.8 . . ?
N5 C8 C7 108.5 . . ?
C7 C8 H8 125.8 . . ?
C8 C7 H7 126.1 . . ?
N6 C7 C8 107.7 . . ?
N6 C7 H7 126.1 . . ?
C9 N6 H6A 126.0 . . ?
C7 N6 C9 108.0 . . ?
C7 N6 H6A 126.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 N2 C1 N1 0.0 . . . . ?
N2 C3 C2 N1 0.0 . . . . ?
N2 C1 N1 C2 0.0 . . . . ?
C1 N1 C2 C3 0.0 . . . . ?
C2 C3 N2 C1 0.0 . . . . ?
N3 C6 N4 C5 0.0 . . . . ?
C6 N3 C4 C5 0.0 . . . . ?
C6 N4 C5 C4 0.0 . . . . ?
N4 C5 C4 N3 0.0 . . . . ?
C4 N3 C6 N4 0.0 . . . . ?
C9 N5 C8 C7 0.0 . . . . ?
N5 C9 N6 C7 0.0 . . . . ?
N5 C8 C7 N6 0.0 . . . . ?
C8 C7 N6 C9 0.0 . . . . ?
N6 C9 N5 C8 0.0 . . . . ?

loop_
_axis.id
_axis.type
_axis.equipment
_axis.parity
_axis.depends_on
_axis.zero
_axis.vector[1]
_axis.vector[2]
_axis.vector[3]
source . source . . . 0.99999963 0.00000000 0.00085835
omega rotation goniometer -1 . -0.89289000 0.00000000 0.00000000 1.00000000
kappa rotation goniometer -1 omega -0.30231000 -0.76666919 0.00000000
0.64204233
phi rotation goniometer -1 kappa . 0.00032376 0.00000000 0.99999995
theta rotation goniometer -1 . -0.80108000 0.00000000 0.00000000 1.00000000
matrixX general general . phi . 1.00000000 0.00000000 0.00000000
matrixY general general . phi . 0.00000000 1.00000000 0.00000000
matrixZ general general . phi . 0.00000000 0.00000000 1.00000000
dacX translation general . phi . 0.00000000 1.00000000 0.00000000
dacY translation general . phi . -1.00000000 0.00000000 0.00000000
dacZ translation general . phi . 0.00000000 0.00000000 1.00000000

_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 13.484
_oxdiff_exptl_absorpt_empirical_full_min 0.508
####################################################################### 
# 
# 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_im2pbbr4_0_65gpa
_database_code_depnum_ccdc_archive 'CCDC 2473969'
loop_
_audit_author_name
_audit_author_address
'Kinga Roszak'
;Adam Mickiewicz University Poznan
Poland
;
_audit_update_record             
;
2025-07-18 deposited with the CCDC.	2026-03-26 downloaded from the CCDC.
;
_audit_creation_date             2023-04-11
# start Validation Reply Form
_vrf_PLAT027_im2pbbr4_0_65gpa    
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      17.50 Degree
RESPONSE: A full set of data was collected, however 
the very high angle data was poor and was omitted.
Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the 
X-ray radiation to the measured sample.
;
_vrf_PLAT029_im2pbbr4_0_65gpa    
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.302 Why?  
RESPONSE: The data come from high-pressure studies and are 
limited by the DAC opening angle.
;
_vrf_PLAT088_im2pbbr4_0_65gpa    
;
PROBLEM: Poor Data / Parameter Ratio ....................       5.11 Note  
RESPONSE: The data/parameter ratio is affected by the access limits of the DAC.
;
_vrf_PLAT342_im2pbbr4_0_65gpa    
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............      0.075 Ang.  
RESPONSE: Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the X-ray 
radiation to the measured sample; poor quality of measurement
;
_vrf_PLAT911_im2pbbr4_0_65gpa    
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        698 Report
RESPONSE: These reflections were probably affected 
by unexpected deviations in their intensities for symmetry 
equivalent measurements and omitted during initial data reduction.
;
# end Validation Reply Form
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br4 Pb, 2(C3 H5 N2)'
_chemical_formula_sum            'C6 H10 Br4 N4 Pb'
_chemical_formula_weight         665.01
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   6.0024(9)
_cell_length_b                   9.245(3)
_cell_length_c                   13.363(8)
_cell_angle_alpha                74.11(4)
_cell_angle_beta                 85.77(4)
_cell_angle_gamma                87.953(19)
_cell_volume                     711.2(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    505
_cell_measurement_temperature    293(2)
_cell_measurement_pressure       690000
_cell_measurement_theta_max      22.6070
_cell_measurement_theta_min      2.2120
_shelx_estimated_absorpt_T_max   0.338
_shelx_estimated_absorpt_T_min   0.076
_exptl_absorpt_coefficient_mu    23.075
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.3481
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.89a (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_density_diffrn    3.105
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1684
_diffrn_reflns_av_unetI/netI     0.1475
_diffrn_reflns_Laue_measured_fraction_full 0.302
_diffrn_reflns_Laue_measured_fraction_max 0.182
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            3136
_diffrn_reflns_point_group_measured_fraction_full 0.302
_diffrn_reflns_point_group_measured_fraction_max 0.182
_diffrn_reflns_theta_full        17.500
_diffrn_reflns_theta_max         27.784
_diffrn_reflns_theta_min         2.291
_diffrn_ambient_temperature      293(2)
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            EosS2
_diffrn_detector_area_resol_mean 16.0338
_diffrn_measured_fraction_theta_full 0.302
_diffrn_measured_fraction_theta_max 0.182
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0015432000
_diffrn_orient_matrix_UB_12      0.0184570000
_diffrn_orient_matrix_UB_13      0.0481935000
_diffrn_orient_matrix_UB_21      0.0287496000
_diffrn_orient_matrix_UB_22      -0.0755410000
_diffrn_orient_matrix_UB_23      0.0254230000
_diffrn_orient_matrix_UB_31      0.1149575000
_diffrn_orient_matrix_UB_32      0.0178091000
_diffrn_orient_matrix_UB_33      -0.0095097000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     28.00  47.50   0.75   20.00    --  -25.07-135.00  57.00   26
  2  ω    -12.00   9.00   0.75   20.00    --  -25.07 -53.00  17.00   28
  3  ω    -42.00 -13.50   0.75   20.00    --  -25.07  19.00   0.00   38
  4  ω   -108.00 -87.00   0.75   20.00    --  -25.07-178.00  90.00   28
  5  ω    -17.00  20.50   0.75   20.00    --  -25.07 -39.00  12.00   50
  6  ω   -108.00 -87.00   0.75   20.00    --  -25.07-178.00 -90.00   28
  7  ω     28.00  47.50   0.75   20.00    --  -25.07-135.00-123.00   26
  8  ω    -55.00 -23.50   0.75   20.00    --  -25.07  77.00 -30.00   42
  9  ω    -30.00   0.00   0.75   20.00    --  -25.07   0.00   0.00   40
 10  ω   -114.00 -60.00   0.75   20.00    --  -25.07 178.00 -90.00   72
 11  ω    -17.00  41.50   0.75   20.00    --  -25.07 -19.00-180.00   78
 12  ω    -25.00  33.50   0.75   20.00    --  -25.07 -13.00   3.00   78
 13  ω    -58.00   0.50   0.75   20.00    --  -25.07  81.00 151.00   78
 14  ω     72.00  93.00   0.75   20.00    --   25.61-178.00 -90.00   28
 15  ω    -12.00   9.00   0.75   20.00    --  -25.07 -53.00-162.00   28
 16  ω    -87.00 -28.50   0.75   20.00    --  -25.07 135.00 123.00   78
 17  ω    -17.00  20.50   0.75   20.00    --  -25.07 -39.00-167.00   50
 18  ω    -40.00  -7.00   0.75   20.00    --  -25.07  57.00 150.00   44
 19  ω    -17.00   7.00   0.75   20.00    --  -25.07 -57.00-150.00   32
 20  ω    -74.00 -15.50   0.75   20.00    --  -25.07 114.00 -45.00   78
 21  ω     -6.00  22.50   0.75   20.00    --  -25.07 -38.00-180.00   38
 22  ω    -30.00  30.00   0.75   20.00    --  -25.07   0.00-180.00   80
 23  ω    -55.00 -23.50   0.75   20.00    --  -25.07  77.00 150.00   42
 24  ω    -17.00  11.50   0.75   20.00    --   25.61 -19.00  30.00   38
 25  ω    -21.00  16.50   0.75   20.00    --   25.61  39.00 -12.00   50
 26  ω    -22.00  24.50   0.75   20.00    --  -25.07 -26.00   8.00   62
 27  ω    -21.00 -18.75   0.75   20.00    --   25.61  39.00 167.00    3
;
_diffrn_measurement_method       'ω scans'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                365
_reflns_number_total             613
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.819
_refine_diff_density_min         -0.871
_refine_diff_density_rms         0.181
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         613
_refine_ls_number_restraints     152
_refine_ls_R_factor_all          0.1350
_refine_ls_R_factor_gt           0.0656
_refine_ls_restrained_S_all      0.913
_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)+(0.0793P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1365
_refine_ls_wR_factor_ref         0.1657
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Rigid bond restraints
 N1, C2, N2, C3, C1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N3, C4, C5, C6, N4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C2 \\sim N2 \\sim C3 \\sim C1 \\sim N1: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
C4 \\sim C6 \\sim N4 \\sim C5 \\sim N3: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Uanis(N2) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C1) \\sim
Ueq, Uanis(C3) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of
0.008
Uanis(C4) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C5) \\sim
Ueq, Uanis(N4) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of
0.008
Uanis(Br3) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(Br2) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
4.a :
 C2(N2,C3,C1,N1), C4(N3,C5,N4,C6)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), N2(H2A), C3(H3), C1(H1), N1(H1A), C4(H4), N3(H3A), C5(H5), N4(H4A),
 C6(H6)
;
_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 0.5106(2) 0.5738(3) 0.3286(5) 0.064(8) Uani 1 1 d . . . . .
Br1 Br 0.4940(7) 0.7263(6) 0.5001(13) 0.088(18) Uani 1 1 d . . . . .
Br2 Br 0.0107(6) 0.5690(6) 0.3300(11) 0.049(3) Uani 1 1 d . U . . .
Br3 Br 0.5099(7) 0.8677(6) 0.1746(13) 0.051(4) Uani 1 1 d . U . . .
Br4 Br 0.5301(7) 0.4109(7) 0.1630(14) 0.08(2) Uani 1 1 d . . . . .
C2 C 0.975(7) 0.642(4) 0.076(7) 0.109(11) Uani 1 1 d G U . . .
H2 H 0.965134 0.556990 0.132928 0.131 Uiso 1 1 calc R U . . .
N2 N 1.139(6) 0.752(5) 0.056(7) 0.110(11) Uani 1 1 d G U . . .
H2A H 1.247741 0.753385 0.094593 0.132 Uiso 1 1 calc R U . . .
C3 C 1.093(8) 0.859(5) -0.037(7) 0.109(11) Uani 1 1 d G U . . .
H3 H 1.175960 0.944712 -0.068361 0.131 Uiso 1 1 calc R U . . .
C1 C 0.901(7) 0.815(5) -0.075(7) 0.104(11) Uani 1 1 d G U . . .
H1 H 0.834906 0.866723 -0.135677 0.125 Uiso 1 1 calc R U . . .
N1 N 0.828(6) 0.681(5) -0.005(7) 0.107(11) Uani 1 1 d G U . . .
H1A H 0.713638 0.630902 -0.010525 0.128 Uiso 1 1 calc R U . . .
C4 C 0.065(6) 0.174(4) 0.363(7) 0.070(9) Uani 1 1 d G U . . .
H4 H 0.112380 0.267635 0.364264 0.084 Uiso 1 1 calc R U . . .
N3 N -0.115(6) 0.146(4) 0.328(7) 0.074(8) Uani 1 1 d G U . . .
H3A H -0.214758 0.211455 0.301349 0.089 Uiso 1 1 calc R U . . .
C5 C -0.121(5) 0.004(4) 0.340(7) 0.073(9) Uani 1 1 d G U . . .
H5 H -0.235144 -0.045950 0.320565 0.088 Uiso 1 1 calc R U . . .
N4 N 0.055(5) -0.056(4) 0.382(6) 0.073(8) Uani 1 1 d G U . . .
H4A H 0.089586 -0.150030 0.397381 0.088 Uiso 1 1 calc R U . . .
C6 C 0.170(6) 0.049(4) 0.396(7) 0.073(9) Uani 1 1 d G U . . .
H6 H 0.306951 0.036332 0.425630 0.087 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br1 3.00(2) . ?
Pb1 Br1 3.075(7) 2_666 ?
Pb1 Br2 3.001(4) 1_655 ?
Pb1 Br2 3.002(4) . ?
Pb1 Br3 2.925(7) . ?
Pb1 Br4 2.99(2) . ?
C2 H2 0.9300 . ?
C2 N2 1.40(3) . ?
C2 N1 1.41(3) . ?
N2 H2A 0.8600 . ?
N2 C3 1.40(3) . ?
C3 H3 0.9300 . ?
C3 C1 1.41(3) . ?
C1 H1 0.9300 . ?
C1 N1 1.40(3) . ?
N1 H1A 0.8600 . ?
C4 H4 0.9300 . ?
C4 N3 1.27(3) . ?
C4 C6 1.28(3) . ?
N3 H3A 0.8600 . ?
N3 C5 1.28(3) . ?
C5 H5 0.9300 . ?
C5 N4 1.27(3) . ?
N4 H4A 0.8600 . ?
N4 C6 1.27(3) . ?
C6 H6 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br1 Pb1 Br1 87.1(3) . 2_666 ?
Br1 Pb1 Br2 92.6(3) . . ?
Br1 Pb1 Br4 177.9(2) . . ?
Br2 Pb1 Br1 88.0(3) 1_655 . ?
Br2 Pb1 Br1 90.01(15) . 2_666 ?
Br2 Pb1 Br1 88.45(15) 1_655 2_666 ?
Br2 Pb1 Br2 178.35(17) 1_655 . ?
Br2 Pb1 Br4 91.6(3) 1_655 . ?
Br2 Pb1 Br4 87.8(3) . . ?
Br3 Pb1 Br1 89.8(4) . . ?
Br3 Pb1 Br1 176.9(5) . 2_666 ?
Br3 Pb1 Br2 91.95(15) . 1_655 ?
Br3 Pb1 Br2 89.62(15) . . ?
Br3 Pb1 Br4 92.2(4) . . ?
Br4 Pb1 Br1 90.9(4) . 2_666 ?
Pb1 Br1 Pb1 92.9(3) . 2_666 ?
Pb1 Br2 Pb1 178.35(17) 1_455 . ?
N2 C2 H2 125.8 . . ?
N2 C2 N1 108.4 . . ?
N1 C2 H2 125.8 . . ?
C2 N2 H2A 126.3 . . ?
C2 N2 C3 107.4 . . ?
C3 N2 H2A 126.3 . . ?
N2 C3 H3 125.7 . . ?
N2 C3 C1 108.6 . . ?
C1 C3 H3 125.7 . . ?
C3 C1 H1 126.2 . . ?
N1 C1 C3 107.7 . . ?
N1 C1 H1 126.2 . . ?
C2 N1 H1A 126.0 . . ?
C1 N1 C2 107.9 . . ?
C1 N1 H1A 126.0 . . ?
N3 C4 H4 126.1 . . ?
N3 C4 C6 107.8 . . ?
C6 C4 H4 126.1 . . ?
C4 N3 H3A 126.1 . . ?
C4 N3 C5 107.8 . . ?
C5 N3 H3A 126.1 . . ?
N3 C5 H5 125.8 . . ?
N4 C5 N3 108.5 . . ?
N4 C5 H5 125.8 . . ?
C5 N4 H4A 126.3 . . ?
C5 N4 C6 107.4 . . ?
C6 N4 H4A 126.3 . . ?
C4 C6 H6 125.7 . . ?
N4 C6 C4 108.5 . . ?
N4 C6 H6 125.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 N2 C3 C1 0.0 . . . . ?
N2 C2 N1 C1 0.1 . . . . ?
N2 C3 C1 N1 0.0 . . . . ?
C3 C1 N1 C2 0.0 . . . . ?
N1 C2 N2 C3 -0.1 . . . . ?
C4 N3 C5 N4 0.0 . . . . ?
N3 C4 C6 N4 0.0 . . . . ?
N3 C5 N4 C6 0.0 . . . . ?
C5 N4 C6 C4 0.0 . . . . ?
C6 C4 N3 C5 0.0 . . . . ?

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

data_impbbr3_429gpa
_database_code_depnum_ccdc_archive 'CCDC 2473967'
loop_
_audit_author_name
_audit_author_address
'Kinga Roszak'
;Adam Mickiewicz University Poznan
Poland
;
_audit_update_record             
;
2025-07-18 deposited with the CCDC.	2026-03-26 downloaded from the CCDC.
;
_audit_creation_date             2025-04-15
# start Validation Reply Form
_vrf_PLAT027_impbbr3_429gpa      
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      17.50 Degree
RESPONSE: A full set of data was collected, however 
the very high angle data was poor and was omitted.
Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the 
X-ray radiation to the measured sample.
;
_vrf_PLAT029_impbbr3_429gpa      
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.464 Why?  
RESPONSE: The data come from high-pressure studies and are 
limited by the DAC opening angle.
;
_vrf_PLAT090_impbbr3_429gpa      
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       4.08 Note  
RESPONSE: The data/parameter ratio is affected by the access limits of the DAC.
;
_vrf_PLAT342_impbbr3_429gpa      
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............      0.045 Ang.  
RESPONSE: Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the X-ray 
radiation to the measured sample; poor quality of measurement
;
_vrf_PLAT910_impbbr3_429gpa      
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         11 Note  
RESPONSE: These reflections were probably affected 
by unexpected deviations in their intensities for symmetry 
equivalent measurements and omitted during initial data reduction.
;
_vrf_PLAT911_impbbr3_429gpa      
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        152 Report
RESPONSE: These reflections were probably affected 
by unexpected deviations in their intensities for symmetry 
equivalent measurements and omitted during initial data reduction.
;
_vrf_PLAT987_impbbr3_429gpa      
;
PROBLEM: The Flack x is >> 0 -  Do a BASF/TWIN Refinement     Please Check 
RESPONSE: The structure was refined as an inversion twin.
;
# end Validation Reply Form
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br3 Pb, C3 H5 N2'
_chemical_formula_sum            'C3 H5 Br3 N2 Pb'
_chemical_formula_weight         516.01
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z+1/2'

_cell_length_a                   13.086(5)
_cell_length_b                   8.2602(4)
_cell_length_c                   14.2630(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1541.7(6)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    2198
_cell_measurement_pressure       4290000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.6350
_cell_measurement_theta_min      4.9240
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    37.349
_exptl_absorpt_correction_T_min  0.41918
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    4.446
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0741
_diffrn_reflns_av_unetI/netI     0.0696
_diffrn_reflns_Laue_measured_fraction_full 0.464
_diffrn_reflns_Laue_measured_fraction_max 0.350
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6861
_diffrn_reflns_point_group_measured_fraction_full 0.471
_diffrn_reflns_point_group_measured_fraction_max 0.353
_diffrn_reflns_theta_full        17.500
_diffrn_reflns_theta_max         26.816
_diffrn_reflns_theta_min         4.936
_diffrn_ambient_temperature      293(2)
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_detector_area_resol_mean 16.2413
_diffrn_measured_fraction_theta_full 0.464
_diffrn_measured_fraction_theta_max 0.350
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0527909544
_diffrn_orient_matrix_UB_12      -0.0198447053
_diffrn_orient_matrix_UB_13      -0.0015203253
_diffrn_orient_matrix_UB_21      -0.0091375017
_diffrn_orient_matrix_UB_22      -0.0521833320
_diffrn_orient_matrix_UB_23      -0.0385342332
_diffrn_orient_matrix_UB_31      0.0086580612
_diffrn_orient_matrix_UB_32      0.0652089431
_diffrn_orient_matrix_UB_33      -0.0313244741
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  19.75   0.75   35.00   0.00 -30.00   0.00    --    73
  2  φ    140.00 200.00   0.75   35.00   0.00 -30.00   0.00    --    80
  3  φ    160.00 217.00   0.75   35.00   0.00  30.00   0.00    --    76
  4  φ    -20.00  34.75   0.75   35.00   0.00  30.00   0.00    --    73
  5  ω    -24.00  24.00   0.75   35.00    --   30.00  39.46 -12.90   64
  6  ω    -24.00  24.00   0.75   35.00    --   30.00  39.46 167.10   64
  7  ω    -50.00  10.00   0.75   35.00    --  -30.00  39.46 167.10   80
  8  ω    -50.00  10.00   0.75   35.00    --  -30.00  39.46 -12.90   80
  9  ω    -64.00  -8.50   0.75   35.00    --  -30.00  81.40 -28.90   74
 10  ω    -64.00  -8.50   0.75   35.00    --  -30.00  81.40 151.10   74
 11  ω    -19.00   8.00   0.75   35.00    --   30.00  81.40 151.10   36
 12  ω    -19.00   8.00   0.75   35.00    --   30.00  81.40 -28.90   36
 13  ω    -43.00 -21.25   0.75   35.00    --   30.00 134.60 -56.90   29
 14  ω    -43.00 -21.25   0.75   35.00    --   30.00 134.60 123.10   29
 15  ω    -90.00 -36.00   0.75   35.00    --  -30.00 134.60 123.10   72
 16  ω    -90.00 -36.00   0.75   35.00    --  -30.00 134.60 -56.90   72
;
_diffrn_measurement_method       'ω and φ scans'
_reflns_Friedel_coverage         0.934
_reflns_Friedel_fraction_full    0.478
_reflns_Friedel_fraction_max     0.355
_reflns_number_gt                945
_reflns_number_total             1139
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.807
_refine_diff_density_min         -0.896
_refine_diff_density_rms         0.211
_refine_ls_abs_structure_details 
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack   0.5
_refine_ls_extinction_coef       0.00023(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         1139
_refine_ls_number_restraints     171
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0368
_refine_ls_restrained_S_all      0.970
_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)+(0.0182P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0592
_refine_ls_wR_factor_ref         0.0657
_refine_special_details          
;
 Refined as a 2-component perfect inversion twin.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Rigid bond restraints
 C5, N4, C4, N3, C6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C1, N1, C2, N2, C3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Br1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Br5, Br3, Br6, Br2, Br4, Br1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
N4 \\sim C4 \\sim N3 \\sim C6 \\sim C5: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
N1 \\sim C2 \\sim N2 \\sim C3 \\sim C1: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
C1 \\sim N1 \\sim C2 \\sim N2 \\sim C3: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Br1: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Br3 \\sim Br6 \\sim Br4 \\sim Br2 \\sim Br5 \\sim Br1: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(Br1) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(N4) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C6) \\sim
Ueq, Uanis(C5) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of
0.008
Uanis(C1) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C2) \\sim
Ueq, Uanis(N1) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of
0.008
Uanis(Pb2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(Br3) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(Br5) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4.a :
 C3(C1,N1,C2,N2), C6(C5,N4,C4,N3)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C1(H1), N1(H1A), C2(H2), N2(H2A), C6(H6), C5(H5), N4(H4), C4(H4A),
 N3(H3A)
;
_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 0.1647(3) -0.01647(17) 0.36745(8) 0.025(2) Uani 1 1 d . . . . .
Pb2 Pb 0.1893(3) 0.00428(15) 0.62601(8) 0.0169(7) Uani 1 1 d . U . . .
Br1 Br 0.2298(9) 0.2617(4) 0.2598(3) 0.021(2) Uani 1 1 d . U . . .
Br2 Br 0.0622(7) 0.2045(4) 0.4993(3) 0.018(5) Uani 1 1 d . . . . .
Br3 Br 0.0090(9) -0.0178(4) 0.7363(3) 0.0269(12) Uani 1 1 d . U . . .
Br4 Br 0.3457(8) 0.0425(4) 0.4723(2) 0.025(6) Uani 1 1 d . . . . .
Br5 Br 0.1238(7) -0.2778(4) 0.5140(2) 0.0219(13) Uani 1 1 d . U . . .
Br6 Br 0.2038(8) 0.3091(4) 0.7339(3) 0.034(6) Uani 1 1 d . . . . .
C3 C 0.384(4) 0.630(3) 0.4452(19) 0.017(7) Uani 1 1 d G U . . .
H3 H 0.416749 0.701366 0.404965 0.020 Uiso 1 1 calc R U . . .
C1 C 0.380(4) 0.642(3) 0.5355(18) 0.021(7) Uani 1 1 d G U . . .
H1 H 0.408549 0.723794 0.571345 0.025 Uiso 1 1 calc R U . . .
N1 N 0.329(4) 0.522(3) 0.5669(16) 0.024(7) Uani 1 1 d G U . . .
H1A H 0.314954 0.502740 0.624776 0.028 Uiso 1 1 calc R U . . .
C2 C 0.302(4) 0.436(2) 0.4960(19) 0.020(7) Uani 1 1 d G U . . .
H2 H 0.263488 0.341548 0.498732 0.024 Uiso 1 1 calc R U . . .
N2 N 0.336(4) 0.503(3) 0.4208(17) 0.021(7) Uani 1 1 d G U . . .
H2A H 0.327765 0.467656 0.364467 0.026 Uiso 1 1 calc R U . . .
C6 C 0.528(4) 0.039(3) 0.3075(19) 0.020(7) Uani 1 1 d G U . . .
H6 H 0.521958 0.090505 0.365323 0.024 Uiso 1 1 calc R U . . .
C5 C 0.580(4) -0.079(3) 0.2889(19) 0.023(8) Uani 1 1 d G U . . .
H5 H 0.621121 -0.136260 0.330561 0.028 Uiso 1 1 calc R U . . .
N4 N 0.567(4) -0.113(3) 0.1987(18) 0.034(7) Uani 1 1 d G U . . .
H4 H 0.595875 -0.191893 0.169761 0.040 Uiso 1 1 calc R U . . .
C4 C 0.507(4) -0.015(3) 0.1614(18) 0.028(8) Uani 1 1 d G U . . .
H4A H 0.484912 -0.011499 0.099398 0.033 Uiso 1 1 calc R U . . .
N3 N 0.483(4) 0.079(3) 0.2287(18) 0.046(8) Uani 1 1 d G U . . .
H3A H 0.441816 0.159657 0.223136 0.055 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br1 2.892(5) . ?
Pb1 Br2 2.944(6) . ?
Pb1 Br3 2.958(10) 2_554 ?
Pb1 Br4 2.843(10) . ?
Pb1 Br5 3.052(4) . ?
Pb1 Br6 2.943(7) 4_544 ?
Pb2 Br1 2.962(6) 4_545 ?
Pb2 Br2 2.960(6) . ?
Pb2 Br3 2.841(10) . ?
Pb2 Br4 3.016(8) . ?
Pb2 Br5 2.952(5) . ?
Pb2 Br6 2.957(4) . ?
C3 H3 0.9300 . ?
C3 C1 1.294(17) . ?
C3 N2 1.271(17) . ?
C1 H1 0.9300 . ?
C1 N1 1.271(17) . ?
N1 H1A 0.8600 . ?
N1 C2 1.285(17) . ?
C2 H2 0.9300 . ?
C2 N2 1.285(17) . ?
N2 H2A 0.8600 . ?
C6 H6 0.9300 . ?
C6 C5 1.22(2) . ?
C6 N3 1.31(2) . ?
C5 H5 0.9300 . ?
C5 N4 1.33(2) . ?
N4 H4 0.8600 . ?
N4 C4 1.25(2) . ?
C4 H4A 0.9300 . ?
C4 N3 1.28(2) . ?
N3 H3A 0.8600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br1 Pb1 Br2 88.90(15) . . ?
Br1 Pb1 Br3 79.3(2) . 2_554 ?
Br1 Pb1 Br5 167.7(2) . . ?
Br1 Pb1 Br6 82.70(18) . 4_544 ?
Br2 Pb1 Br3 89.7(2) . 2_554 ?
Br2 Pb1 Br5 85.47(15) . . ?
Br3 Pb1 Br5 111.5(2) 2_554 . ?
Br4 Pb1 Br1 84.1(2) . . ?
Br4 Pb1 Br2 86.4(2) . . ?
Br4 Pb1 Br3 163.05(14) . 2_554 ?
Br4 Pb1 Br5 84.7(2) . . ?
Br4 Pb1 Br6 86.4(2) . 4_544 ?
Br6 Pb1 Br2 169.4(2) 4_544 . ?
Br6 Pb1 Br3 95.0(2) 4_544 2_554 ?
Br6 Pb1 Br5 101.51(15) 4_544 . ?
Br1 Pb2 Br4 107.3(2) 4_545 . ?
Br2 Pb2 Br1 166.3(3) . 4_545 ?
Br2 Pb2 Br4 83.0(2) . . ?
Br3 Pb2 Br1 84.1(3) . 4_545 ?
Br3 Pb2 Br2 84.7(2) . . ?
Br3 Pb2 Br4 166.6(2) . . ?
Br3 Pb2 Br5 90.4(2) . . ?
Br3 Pb2 Br6 79.6(2) . . ?
Br5 Pb2 Br1 85.32(14) . 4_545 ?
Br5 Pb2 Br2 87.00(17) . . ?
Br5 Pb2 Br4 83.46(18) . . ?
Br5 Pb2 Br6 166.5(3) . . ?
Br6 Pb2 Br1 102.57(15) . 4_545 ?
Br6 Pb2 Br2 83.00(16) . . ?
Br6 Pb2 Br4 104.22(19) . . ?
Pb1 Br1 Pb2 169.9(2) . 4_554 ?
Pb1 Br2 Pb2 77.75(17) . . ?
Pb2 Br3 Pb1 169.2(2) . 2 ?
Pb1 Br4 Pb2 78.4(3) . . ?
Pb2 Br5 Pb1 76.21(11) . . ?
Pb1 Br6 Pb2 142.3(3) 4 . ?
C1 C3 H3 125.8 . . ?
N2 C3 H3 125.8 . . ?
N2 C3 C1 108.3 . . ?
C3 C1 H1 125.8 . . ?
N1 C1 C3 108.3 . . ?
N1 C1 H1 125.8 . . ?
C1 N1 H1A 126.4 . . ?
C1 N1 C2 107.2 . . ?
C2 N1 H1A 126.4 . . ?
N1 C2 H2 125.5 . . ?
N1 C2 N2 109.0 . . ?
N2 C2 H2 125.5 . . ?
C3 N2 C2 107.1 . . ?
C3 N2 H2A 126.4 . . ?
C2 N2 H2A 126.4 . . ?
C5 C6 H6 127.3 . . ?
C5 C6 N3 105.3 . . ?
N3 C6 H6 127.3 . . ?
C6 C5 H5 126.1 . . ?
C6 C5 N4 107.9 . . ?
N4 C5 H5 126.1 . . ?
C5 N4 H4 124.5 . . ?
C4 N4 C5 111.1 . . ?
C4 N4 H4 124.5 . . ?
N4 C4 H4A 128.4 . . ?
N4 C4 N3 103.2 . . ?
N3 C4 H4A 128.4 . . ?
C6 N3 H3A 123.8 . . ?
C4 N3 C6 112.5 . . ?
C4 N3 H3A 123.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 C1 N1 C2 0.0 . . . . ?
C1 C3 N2 C2 0.0 . . . . ?
C1 N1 C2 N2 0.1 . . . . ?
N1 C2 N2 C3 -0.1 . . . . ?
N2 C3 C1 N1 0.0 . . . . ?
C6 C5 N4 C4 0.0 . . . . ?
C5 C6 N3 C4 0.0 . . . . ?
C5 N4 C4 N3 0.0 . . . . ?
N4 C4 N3 C6 0.0 . . . . ?
N3 C6 C5 N4 0.0 . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'

# end
####################################################################### 
# 
# 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_im2pbbr4_4_13gpa
_database_code_depnum_ccdc_archive 'CCDC 2473976'
loop_
_audit_author_name
_audit_author_address
'Kinga Roszak'
;Adam Mickiewicz University Poznan
Poland
;
_audit_update_record             
;
2025-07-18 deposited with the CCDC.	2026-03-26 downloaded from the CCDC.
;
_audit_creation_date             2023-07-13
# start Validation Reply Form
_vrf_RINTA01_im2pbbr4_4_13gpa    
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: High factor is a result from the weak diffraction. Due to the specificity 
of the applied measuring technique and use of a diamond-anvil cell 
limiting the access of the X-ray radiation to the measured sample.
;
_vrf_PLAT027_im2pbbr4_4_13gpa    
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      17.50 Degree
RESPONSE: A full set of data was collected, however 
the very high angle data was poor and was omitted.
Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the 
X-ray radiation to the measured sample.
;
_vrf_PLAT029_im2pbbr4_4_13gpa    
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.308 Why?  
RESPONSE: The data come from high-pressure studies and are 
limited by the DAC opening angle.
;
_vrf_PLAT088_im2pbbr4_4_13gpa    
;
PROBLEM: Poor Data / Parameter Ratio ....................       4.31 Note  
RESPONSE: The data/parameter ratio is affected by the access limits of the DAC.
;
_vrf_PLAT020_im2pbbr4_4_13gpa    
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.196 Report
RESPONSE: High factor is a result from the weak diffraction. Due to the specificity 
of the applied measuring technique and use of a diamond-anvil cell 
limiting the access of the X-ray radiation to the measured sample.
;
_vrf_PLAT342_im2pbbr4_4_13gpa    
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............      0.075 Ang.  
RESPONSE: Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the X-ray 
radiation to the measured sample; poor quality of measurement
;
_vrf_PLAT911_im2pbbr4_4_13gpa    
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        484 Report
RESPONSE: These reflections were probably affected 
by unexpected deviations in their intensities for symmetry 
equivalent measurements and omitted during initial data reduction.
;
# end Validation Reply Form
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br4 Pb, 2(C3 H5 N2)'
_chemical_formula_sum            'C6 H10 Br4 N4 Pb'
_chemical_formula_weight         665.01
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   5.749(4)
_cell_length_b                   9.075(7)
_cell_length_c                   12.356(16)
_cell_angle_alpha                71.40(12)
_cell_angle_beta                 81.78(12)
_cell_angle_gamma                85.02(6)
_cell_volume                     604.1(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    496
_cell_measurement_pressure       4130000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.2970
_cell_measurement_theta_min      3.4760
_shelx_estimated_absorpt_T_max   0.293
_shelx_estimated_absorpt_T_min   0.062
_exptl_absorpt_coefficient_mu    27.165
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8114
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.89a (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_density_diffrn    3.656
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1956
_diffrn_reflns_av_unetI/netI     0.2291
_diffrn_reflns_Laue_measured_fraction_full 0.308
_diffrn_reflns_Laue_measured_fraction_max 0.169
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            3244
_diffrn_reflns_point_group_measured_fraction_full 0.308
_diffrn_reflns_point_group_measured_fraction_max 0.169
_diffrn_reflns_theta_full        17.500
_diffrn_reflns_theta_max         28.522
_diffrn_reflns_theta_min         2.370
_diffrn_ambient_temperature      293(2)
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_detector_area_resol_mean 16.1544
_diffrn_measured_fraction_theta_full 0.308
_diffrn_measured_fraction_theta_max 0.169
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0137675000
_diffrn_orient_matrix_UB_12      0.0046747000
_diffrn_orient_matrix_UB_13      0.0567982000
_diffrn_orient_matrix_UB_21      0.0316872000
_diffrn_orient_matrix_UB_22      -0.0804195000
_diffrn_orient_matrix_UB_23      0.0212464000
_diffrn_orient_matrix_UB_31      0.1198999000
_diffrn_orient_matrix_UB_32      0.0180228000
_diffrn_orient_matrix_UB_33      -0.0068513000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -3.00  19.40   0.70   14.00    --   17.94  57.00 -30.00   32
  2  ω    -31.00   0.50   0.70   14.00    --   17.94   0.00-150.00   45
  3  ω     -8.00  43.10   0.70   14.00    --   17.94 -37.00-180.00   73
  4  ω    -34.00  26.20   0.70   14.00    --   17.94  13.00  -3.00   86
  5  ω    -20.00   2.40   0.70   14.00    --  -18.72 -57.00-150.00   32
  6  ω    -23.00  13.40   0.70   14.00    --  -18.72 -26.00-172.00   52
  7  ω    -81.00 -25.00   0.70   14.00    --  -18.72 134.00 -56.00   80
  8  ω    -23.00  13.40   0.70   14.00    --  -18.72 -26.00   7.00   52
  9  ω    -44.00  18.30   0.70   14.00    --  -18.72  39.00 167.00   89
 10  ω    -81.00 -25.00   0.70   14.00    --  -18.72 134.00 123.00   80
 11  ω    -20.00   2.40   0.70   14.00    --  -18.72 -57.00  30.00   32
 12  ω    -44.00  18.30   0.70   14.00    --  -18.72  39.00 -12.00   89
 13  ω      4.00  39.00   0.70   14.00    --   17.94 -57.00  30.00   50
 14  ω     -3.00  19.40   0.70   14.00    --   17.94  57.00 150.00   32
 15  ω    -12.70   9.00   0.70   14.00    --   17.94  77.00 -60.00   31
 16  ω    -26.00  17.40   0.70   14.00    --   17.94  19.00-180.00   62
 17  ω      4.00  39.00   0.70   14.00    --   17.94 -57.00-150.00   50
 18  ω    -45.00 -25.40   0.70   14.00    --  -18.72  37.00   0.00   28
 19  ω    -19.00   5.50   0.70   14.00    --  -18.72 -39.00-167.00   35
 20  ω    -43.00   8.10   0.70   14.00    --  -18.72  67.00 157.00   73
 21  ω    -43.00 -11.50   0.70   14.00    --  -18.72  19.00   0.00   45
 22  ω    -19.00   5.50   0.70   14.00    --  -18.72 -39.00  12.00   35
 23  ω    -36.00  26.30   0.70   14.00    --   17.94  13.00 176.00   89
 24  ω    -27.00  35.30   0.70   14.00    --   17.94 -13.00-176.00   89
 25  ω    -19.00  43.30   0.70   14.00    --   17.94 -19.00-180.00   89
 26  ω      9.00  52.40   0.70   14.00    --   17.94 -99.00  30.00   62
 27  ω    -23.00  39.30   0.70   14.00    --   17.94 -26.00   7.00   89
 28  ω    -23.00  39.30   0.70   14.00    --   17.94 -26.00-172.00   89
 29  ω    -59.00  -4.40   0.70   14.00    --  -18.72  97.00 143.00   78
 30  ω    -27.00  35.30   0.70   14.00    --  -18.72 -13.00   3.00   89
 31  ω    -44.00  18.30   0.70   14.00    --  -18.72  19.00-180.00   89
 32  ω    -40.00  13.20   0.70   14.00    --  -18.72  53.00 -17.00   76
 33  ω    -40.00  22.30   0.70   14.00    --  -18.72  26.00  -7.00   89
 34  ω    -44.00  18.30   0.70   14.00    --  -18.72  39.00 -12.00   89
 35  ω    -27.00  -1.80   0.70   14.00    --  -18.72 -13.00-176.00   36
 36  ω    -36.00  26.30   0.70   14.00    --  -18.72  13.00  -3.00   89
;
_diffrn_measurement_method       'ω scans'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                271
_reflns_number_total             517
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.800
_refine_diff_density_min         -0.607
_refine_diff_density_rms         0.190
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         517
_refine_ls_number_restraints     267
_refine_ls_R_factor_all          0.1795
_refine_ls_R_factor_gt           0.0778
_refine_ls_restrained_S_all      0.804
_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)+(0.0995P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1573
_refine_ls_wR_factor_ref         0.1981
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 C3-C2
 2.1 with sigma of 0.02
3. Rigid bond restraints
 C2, N2, C3, C1, N1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Br2, Br1, Br3, Pb1, Br4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C6, C4, N3, C5, N4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C2 \\sim N2 \\sim C3 \\sim C1 \\sim N1: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Br4 \\sim Pb1 \\sim Br1 \\sim Br2 \\sim Br3: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C6 \\sim C4 \\sim N3 \\sim C5 \\sim N4: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Uanis(C2) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C3) \\sim
Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(Br4) \\sim Ueq, Uanis(Pb1) \\sim Ueq, Uanis(Br3) \\sim Ueq, Uanis(Br1)
\\sim Ueq, Uanis(Br2) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C6) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C5) \\sim
Ueq, Uanis(N4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
5. Rigid body (RIGU) restrains
 C2, N2, N1, C3, C1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Br4, Pb1, Br3, Br1, Br2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C6, C4, N3, C5, N4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a :
 C2(N2,C3,C1,N1), C4(N3,C5,N4,C6)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), N2(H2A), C3(H3), C1(H1), N1(H1A), C4(H4), N3(H3A), C5(H5), N4(H4A),
 C6(H6)
;
_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 0.5619(4) 0.5772(2) 0.3166(6) 0.055(4) Uani 1 1 d . U . . .
Br1 Br 0.5088(11) 0.7233(6) 0.4971(16) 0.058(4) Uani 1 1 d . U . . .
Br2 Br 0.0690(10) 0.5984(6) 0.3423(15) 0.050(4) Uani 1 1 d . U . . .
Br3 Br 0.5307(12) 0.8887(6) 0.1634(17) 0.063(5) Uani 1 1 d . U . . .
Br4 Br 0.5233(11) 0.3866(6) 0.1573(17) 0.059(4) Uani 1 1 d . U . . .
C2 C 1.011(8) 0.643(4) 0.067(7) 0.081(13) Uani 1 1 d DG U . . .
H2 H 1.043756 0.552488 0.125500 0.097 Uiso 1 1 calc R U . . .
N2 N 1.125(8) 0.773(5) 0.041(8) 0.083(13) Uani 1 1 d G U . . .
H2A H 1.238286 0.790796 0.072927 0.099 Uiso 1 1 calc R U . . .
C3 C 1.026(9) 0.868(4) -0.045(8) 0.080(13) Uani 1 1 d DG U . . .
H3 H 1.067918 0.970544 -0.082477 0.096 Uiso 1 1 calc R U . . .
C1 C 0.851(9) 0.797(5) -0.071(8) 0.077(13) Uani 1 1 d G U . . .
H1 H 0.755877 0.841768 -0.129210 0.093 Uiso 1 1 calc R U . . .
N1 N 0.842(8) 0.657(4) -0.002(8) 0.078(13) Uani 1 1 d G U . . .
H1A H 0.747677 0.587457 -0.000159 0.094 Uiso 1 1 calc R U . . .
C4 C 0.067(8) 0.187(4) 0.361(10) 0.060(11) Uani 1 1 d G U . . .
H4 H 0.094360 0.282711 0.367235 0.072 Uiso 1 1 calc R U . . .
N3 N -0.133(7) 0.138(4) 0.349(10) 0.062(10) Uani 1 1 d G U . . .
H3A H -0.264216 0.191754 0.346201 0.074 Uiso 1 1 calc R U . . .
C5 C -0.103(8) -0.006(4) 0.342(9) 0.059(11) Uani 1 1 d G U . . .
H5 H -0.219099 -0.065818 0.333989 0.071 Uiso 1 1 calc R U . . .
N4 N 0.115(7) -0.047(4) 0.350(9) 0.058(10) Uani 1 1 d G U . . .
H4A H 0.181059 -0.134826 0.347678 0.069 Uiso 1 1 calc R U . . .
C6 C 0.220(7) 0.072(4) 0.361(11) 0.059(11) Uani 1 1 d G U . . .
H6 H 0.379039 0.073069 0.367911 0.070 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 2.970(11) 2_666 ?
Pb1 Br1 2.91(2) . ?
Pb1 Br2 3.007(7) 1_655 ?
Pb1 Br2 2.803(6) . ?
Pb1 Br3 2.864(9) . ?
Pb1 Br4 3.05(2) . ?
C2 H2 0.9300 . ?
C2 N2 1.329(13) . ?
C2 N1 1.357(13) . ?
N2 H2A 0.8600 . ?
N2 C3 1.299(13) . ?
C3 H3 0.9300 . ?
C3 C1 1.374(14) . ?
C1 H1 0.9300 . ?
C1 N1 1.282(13) . ?
N1 H1A 0.8600 . ?
C4 H4 0.9300 . ?
C4 N3 1.31(3) . ?
C4 C6 1.30(3) . ?
N3 H3A 0.8600 . ?
N3 C5 1.33(3) . ?
C5 H5 0.9300 . ?
C5 N4 1.28(3) . ?
N4 H4A 0.8600 . ?
N4 C6 1.34(3) . ?
C6 H6 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br1 Pb1 Br1 86.9(3) . 2_666 ?
Br1 Pb1 Br2 95.6(2) 2_666 1_655 ?
Br1 Pb1 Br2 79.5(4) . 1_655 ?
Br1 Pb1 Br4 84.5(4) 2_666 . ?
Br1 Pb1 Br4 167.5(3) . . ?
Br2 Pb1 Br1 84.0(4) . . ?
Br2 Pb1 Br1 83.6(2) . 2_666 ?
Br2 Pb1 Br2 163.5(7) . 1_655 ?
Br2 Pb1 Br3 85.1(2) . . ?
Br2 Pb1 Br4 110.3(4) 1_655 . ?
Br2 Pb1 Br4 86.1(4) . . ?
Br3 Pb1 Br1 85.0(4) . . ?
Br3 Pb1 Br1 166.7(4) . 2_666 ?
Br3 Pb1 Br2 93.3(2) . 1_655 ?
Br3 Pb1 Br4 101.7(5) . . ?
Pb1 Br1 Pb1 93.1(3) . 2_666 ?
Pb1 Br2 Pb1 163.5(7) . 1_455 ?
N2 C2 H2 124.1 . . ?
N2 C2 N1 111.8 . . ?
N1 C2 H2 124.1 . . ?
C2 N2 H2A 127.9 . . ?
C3 N2 C2 104.1 . . ?
C3 N2 H2A 127.9 . . ?
N2 C3 H3 124.8 . . ?
N2 C3 C1 110.4 . . ?
C1 C3 H3 124.8 . . ?
C3 C1 H1 126.0 . . ?
N1 C1 C3 108.0 . . ?
N1 C1 H1 126.0 . . ?
C2 N1 H1A 127.2 . . ?
C1 N1 C2 105.6 . . ?
C1 N1 H1A 127.2 . . ?
N3 C4 H4 127.2 . . ?
C6 C4 H4 127.2 . . ?
C6 C4 N3 105.7 . . ?
C4 N3 H3A 125.0 . . ?
C4 N3 C5 110.0 . . ?
C5 N3 H3A 125.0 . . ?
N3 C5 H5 126.5 . . ?
N4 C5 N3 107.0 . . ?
N4 C5 H5 126.5 . . ?
C5 N4 H4A 126.2 . . ?
C5 N4 C6 107.6 . . ?
C6 N4 H4A 126.2 . . ?
C4 C6 N4 109.7 . . ?
C4 C6 H6 125.1 . . ?
N4 C6 H6 125.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 N2 C3 C1 0.0 . . . . ?
N2 C2 N1 C1 0.1 . . . . ?
N2 C3 C1 N1 0.0 . . . . ?
C3 C1 N1 C2 0.0 . . . . ?
N1 C2 N2 C3 -0.1 . . . . ?
C4 N3 C5 N4 -0.1 . . . . ?
N3 C4 C6 N4 -0.1 . . . . ?
N3 C5 N4 C6 0.0 . . . . ?
C5 N4 C6 C4 0.0 . . . . ?
C6 C4 N3 C5 0.1 . . . . ?

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

data_im2pbbr4_2_22gpa
_database_code_depnum_ccdc_archive 'CCDC 2473972'
loop_
_audit_author_name
_audit_author_address
'Kinga Roszak'
;Adam Mickiewicz University Poznan
Poland
;
_audit_update_record             
;
2025-07-18 deposited with the CCDC.	2026-03-26 downloaded from the CCDC.
;
_audit_creation_date             2023-04-14
# start Validation Reply Form
_vrf_RINTA01_im2pbbr4_2_22gpa    
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: High factor is a result from the weak diffraction. Due to the specificity 
of the applied measuring technique and use of a diamond-anvil cell 
limiting the access of the X-ray radiation to the measured sample.
;
_vrf_PLAT027_im2pbbr4_2_22gpa    
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      17.50 Degree
RESPONSE: A full set of data was collected, however 
the very high angle data was poor and was omitted.
Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the 
X-ray radiation to the measured sample.
;
_vrf_PLAT029_im2pbbr4_2_22gpa    
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.294 Why?  
RESPONSE: The data come from high-pressure studies and are 
limited by the DAC opening angle.
;
_vrf_PLAT088_im2pbbr4_2_22gpa    
;
PROBLEM: Poor Data / Parameter Ratio ....................       4.72 Note  
RESPONSE: The data/parameter ratio is affected by the access limits of the DAC.
;
_vrf_PLAT342_im2pbbr4_2_22gpa    
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............       0.05 Ang.  
RESPONSE: Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the X-ray 
radiation to the measured sample; poor quality of measurement
;
_vrf_PLAT911_im2pbbr4_2_22gpa    
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        476 Report
RESPONSE: These reflections were probably affected 
by unexpected deviations in their intensities for symmetry 
equivalent measurements and omitted during initial data reduction.
;
# end Validation Reply Form
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br4 Pb, 2(C3 H5 N2)'
_chemical_formula_sum            'C6 H10 Br4 N4 Pb'
_chemical_formula_weight         665.01
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   5.8790(10)
_cell_length_b                   9.118(3)
_cell_length_c                   12.730(7)
_cell_angle_alpha                73.36(4)
_cell_angle_beta                 84.27(3)
_cell_angle_gamma                87.12(2)
_cell_volume                     650.4(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1005
_cell_measurement_pressure       2220000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.0440
_cell_measurement_theta_min      3.4240
_shelx_estimated_absorpt_T_max   0.313
_shelx_estimated_absorpt_T_min   0.068
_exptl_absorpt_coefficient_mu    25.232
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7134
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.89a (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_density_diffrn    3.396
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1831
_diffrn_reflns_av_unetI/netI     0.1256
_diffrn_reflns_Laue_measured_fraction_full 0.294
_diffrn_reflns_Laue_measured_fraction_max 0.197
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            6784
_diffrn_reflns_point_group_measured_fraction_full 0.294
_diffrn_reflns_point_group_measured_fraction_max 0.197
_diffrn_reflns_theta_full        17.500
_diffrn_reflns_theta_max         27.078
_diffrn_reflns_theta_min         2.332
_diffrn_ambient_temperature      293(2)
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_detector_area_resol_mean 16.1544
_diffrn_measured_fraction_theta_full 0.294
_diffrn_measured_fraction_theta_max 0.197
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0053268000
_diffrn_orient_matrix_UB_12      0.0131699000
_diffrn_orient_matrix_UB_13      0.0524814000
_diffrn_orient_matrix_UB_21      0.0299525000
_diffrn_orient_matrix_UB_22      -0.0779504000
_diffrn_orient_matrix_UB_23      0.0239160000
_diffrn_orient_matrix_UB_31      0.1174091000
_diffrn_orient_matrix_UB_32      0.0185771000
_diffrn_orient_matrix_UB_33      -0.0091016000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -9.00  22.20   0.80   15.00    --   15.75  39.00 -12.00   39
  2  ω    -26.00  22.00   0.80   15.00    --   15.75  19.00-180.00   60
  3  ω    -20.00  46.40   0.80   15.00    --   15.75 -19.00-180.00   83
  4  ω     -6.00  22.80   0.80   15.00    --   15.75  57.00 150.00   36
  5  ω    -26.00  42.00   0.80   15.00    --   15.75 -26.00   7.00   85
  6  ω    -24.00  -1.60   0.80   15.00    --   15.75  97.00 -35.00   28
  7  ω    -79.00 -23.00   0.80   15.00    --  -16.61 134.00 -56.00   70
  8  ω    -41.00  21.40   0.80   15.00    --  -16.61  39.00 -12.00   78
  9  ω    -23.00   8.20   0.80   15.00    --  -16.61 -39.00-167.00   39
 10  ω    -29.00  38.20   0.80   15.00    --  -16.61 -13.00   3.00   84
 11  ω    -23.00   4.20   0.80   15.00    --  -16.61 -57.00-150.00   34
 12  ω    -79.00 -23.00   0.80   15.00    --  -16.61 134.00 123.00   70
 13  ω    -42.00  25.20   0.80   15.00    --  -16.61  26.00 172.00   84
 14  ω    -16.00  26.40   0.80   15.00    --   15.75  26.00  -7.00   53
 15  ω     -9.00  39.00   0.80   15.00    --   15.75 -67.00  23.00   60
 16  ω     -9.00  40.60   0.80   15.00    --   15.75 -37.00-180.00   62
 17  ω     15.00  44.60   0.80   15.00    --   15.75 -77.00-150.00   37
 18  ω    -42.00  10.00   0.80   15.00    --  -16.61  37.00-180.00   65
 19  ω    -21.00  27.00   0.80   15.00    --  -16.61 -19.00-180.00   60
 20  ω    -26.00  16.40   0.80   15.00    --  -16.61 -26.00-172.00   53
 21  ω    -41.00  11.00   0.80   15.00    --  -16.61  67.00 -23.00   65
 22  ω     22.00  43.60   0.80   15.00    --  -16.61-134.00-123.00   27
 23  ω     22.00  43.60   0.80   15.00    --  -16.61-134.00  56.00   27
 24  ω    -29.00  38.20   0.80   15.00    --   15.75 -13.00   3.00   84
 25  ω    -39.00  29.00   0.80   15.00    --   15.75  13.00 176.00   85
 26  ω    -26.00  42.00   0.80   15.00    --   15.75 -26.00   7.00   85
 27  ω    -18.00  41.20   0.80   15.00    --   15.75 -39.00-167.00   74
 28  ω    -38.00  29.20   0.80   15.00    --   15.75  13.00  -3.00   84
 29  ω    -47.00  21.00   0.80   15.00    --  -16.61  19.00-180.00   85
 30  ω    -39.00  -7.00   0.80   15.00    --  -16.61  13.00  -3.00   40
 31  ω    -34.00  34.00   0.80   15.00    --  -16.61   0.00   0.00   85
 32  ω    -29.00  38.20   0.80   15.00    --  -16.61 -13.00   3.00   84
 33  ω    -34.00  34.00   0.80   15.00    --  -16.61   0.00-180.00   85
;
_diffrn_measurement_method       'ω scans'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                334
_reflns_number_total             566
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.894
_refine_diff_density_min         -0.643
_refine_diff_density_rms         0.173
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         566
_refine_ls_number_restraints     147
_refine_ls_R_factor_all          0.1168
_refine_ls_R_factor_gt           0.0615
_refine_ls_restrained_S_all      0.889
_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)+(0.0818P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1293
_refine_ls_wR_factor_ref         0.1543
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 C6-C5
 2.1 with sigma of 0.02
3. Rigid bond restraints
 C6, C4, N3, C5, N4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C2, N1, C1, C3, N2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
N4 \\sim C5 \\sim N3 \\sim C4 \\sim C6: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
N2 \\sim C3 \\sim C1 \\sim N1 \\sim C2: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Uanis(N4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(C6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C3) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(N1) \\sim
Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(Br3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5.a :
 C2(N2,C3,C1,N1), C4(N3,C5,N4,C6)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), N2(H2A), C3(H3), C1(H1), N1(H1A), C4(H4), N3(H3A), C5(H5), N4(H4A),
 C6(H6)
;
_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 0.5183(2) 0.57650(18) 0.3253(4) 0.054(6) Uani 1 1 d . . . . .
Br1 Br 0.4954(6) 0.7302(5) 0.5034(10) 0.044(14) Uani 1 1 d . . . . .
Br2 Br 0.0195(6) 0.5788(5) 0.3355(11) 0.064(14) Uani 1 1 d . . . . .
Br3 Br 0.5141(6) 0.8733(5) 0.1632(11) 0.041(8) Uani 1 1 d . U . . .
Br4 Br 0.5329(6) 0.4037(5) 0.1622(11) 0.083(16) Uani 1 1 d . . . . .
C2 C 1.063(5) 0.674(4) 0.072(6) 0.074(10) Uani 1 1 d G U . . .
H2 H 1.120537 0.595766 0.127800 0.088 Uiso 1 1 calc R U . . .
N2 N 1.146(5) 0.810(4) 0.033(6) 0.070(10) Uani 1 1 d G U . . .
H2A H 1.261952 0.844836 0.054094 0.084 Uiso 1 1 calc R U . . .
C3 C 1.019(5) 0.884(3) -0.044(6) 0.068(10) Uani 1 1 d G U . . .
H3 H 1.037967 0.984628 -0.085871 0.082 Uiso 1 1 calc R U . . .
C1 C 0.857(5) 0.793(4) -0.052(6) 0.054(9) Uani 1 1 d G U . . .
H1 H 0.744004 0.818502 -0.101284 0.065 Uiso 1 1 calc R U . . .
N1 N 0.884(5) 0.663(3) 0.019(6) 0.061(9) Uani 1 1 d G U . . .
H1A H 0.801731 0.583781 0.030487 0.074 Uiso 1 1 calc R U . . .
C4 C 0.081(5) 0.184(3) 0.359(7) 0.057(9) Uani 1 1 d G U . . .
H4 H 0.143328 0.277239 0.355186 0.068 Uiso 1 1 calc R U . . .
N3 N -0.123(4) 0.163(3) 0.338(7) 0.059(9) Uani 1 1 d G U . . .
H3A H -0.226597 0.233014 0.318802 0.070 Uiso 1 1 calc R U . . .
C5 C -0.143(5) 0.014(3) 0.353(7) 0.049(8) Uani 1 1 d DG U . . .
H5 H -0.274321 -0.032093 0.343565 0.059 Uiso 1 1 calc R U . . .
N4 N 0.048(4) -0.057(2) 0.382(6) 0.046(8) Uani 1 1 d G U . . .
H4A H 0.076223 -0.153845 0.396525 0.055 Uiso 1 1 calc R U . . .
C6 C 0.186(4) 0.048(3) 0.386(6) 0.050(9) Uani 1 1 d DG U . . .
H6 H 0.336178 0.030245 0.404706 0.060 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 2.976(15) . ?
Pb1 Br1 3.013(6) 2_666 ?
Pb1 Br2 2.964(4) 1_655 ?
Pb1 Br2 2.922(3) . ?
Pb1 Br3 2.897(6) . ?
Pb1 Br4 2.937(15) . ?
C2 H2 0.9300 . ?
C2 N2 1.30(2) . ?
C2 N1 1.32(2) . ?
N2 H2A 0.8600 . ?
N2 C3 1.30(2) . ?
C3 H3 0.9300 . ?
C3 C1 1.33(2) . ?
C1 H1 0.9300 . ?
C1 N1 1.28(2) . ?
N1 H1A 0.8600 . ?
C4 H4 0.9300 . ?
C4 N3 1.285(11) . ?
C4 C6 1.328(12) . ?
N3 H3A 0.8600 . ?
N3 C5 1.328(12) . ?
C5 H5 0.9300 . ?
C5 N4 1.302(12) . ?
N4 H4A 0.8600 . ?
N4 C6 1.302(12) . ?
C6 H6 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br1 Pb1 Br1 89.6(2) . 2_666 ?
Br2 Pb1 Br1 89.23(15) 1_655 2_666 ?
Br2 Pb1 Br1 90.6(3) . . ?
Br2 Pb1 Br1 84.4(3) 1_655 . ?
Br2 Pb1 Br1 89.09(15) . 2_666 ?
Br2 Pb1 Br2 174.7(6) . 1_655 ?
Br2 Pb1 Br4 88.5(3) . . ?
Br3 Pb1 Br1 89.7(3) . . ?
Br3 Pb1 Br1 177.90(17) . 2_666 ?
Br3 Pb1 Br2 88.94(14) . . ?
Br3 Pb1 Br2 92.67(15) . 1_655 ?
Br3 Pb1 Br4 94.4(3) . . ?
Br4 Pb1 Br1 86.2(3) . 2_666 ?
Br4 Pb1 Br1 175.8(2) . . ?
Br4 Pb1 Br2 96.3(3) . 1_655 ?
Pb1 Br1 Pb1 90.4(2) . 2_666 ?
Pb1 Br2 Pb1 174.7(6) . 1_455 ?
N2 C2 H2 125.1 . . ?
N2 C2 N1 109.7 . . ?
N1 C2 H2 125.1 . . ?
C2 N2 H2A 127.0 . . ?
C3 N2 C2 105.9 . . ?
C3 N2 H2A 127.0 . . ?
N2 C3 H3 125.2 . . ?
N2 C3 C1 109.7 . . ?
C1 C3 H3 125.2 . . ?
C3 C1 H1 126.3 . . ?
N1 C1 C3 107.4 . . ?
N1 C1 H1 126.3 . . ?
C2 N1 H1A 126.4 . . ?
C1 N1 C2 107.3 . . ?
C1 N1 H1A 126.4 . . ?
N3 C4 H4 126.3 . . ?
N3 C4 C6 107.5 . . ?
C6 C4 H4 126.3 . . ?
C4 N3 H3A 126.3 . . ?
C4 N3 C5 107.3 . . ?
C5 N3 H3A 126.3 . . ?
N3 C5 H5 125.2 . . ?
N4 C5 N3 109.6 . . ?
N4 C5 H5 125.2 . . ?
C5 N4 H4A 127.0 . . ?
C6 N4 C5 106.0 . . ?
C6 N4 H4A 127.0 . . ?
C4 C6 H6 125.2 . . ?
N4 C6 C4 109.6 . . ?
N4 C6 H6 125.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 N2 C3 C1 0.0 . . . . ?
N2 C2 N1 C1 0.1 . . . . ?
N2 C3 C1 N1 0.0 . . . . ?
C3 C1 N1 C2 1(7) . . . . ?
N1 C2 N2 C3 -0.1 . . . . ?
C4 N3 C5 N4 0.0 . . . . ?
N3 C4 C6 N4 0.0 . . . . ?
N3 C5 N4 C6 0.0 . . . . ?
C5 N4 C6 C4 0.0 . . . . ?
C6 C4 N3 C5 0.0 . . . . ?

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

data_impbbr3_235gpa
_database_code_depnum_ccdc_archive 'CCDC 2473963'
loop_
_audit_author_name
_audit_author_address
'Kinga Roszak'
;Adam Mickiewicz University Poznan
Poland
;
_audit_update_record             
;
2025-07-18 deposited with the CCDC.	2026-03-26 downloaded from the CCDC.
;
_audit_creation_date             2024-08-01
# start Validation Reply Form
_vrf_PLAT027_impbbr3_235gpa      
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      15.00 Degree
RESPONSE: A full set of data was collected, however 
the very high angle data was poor and was omitted.
Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the 
X-ray radiation to the measured sample.
;
_vrf_PLAT029_impbbr3_235gpa      
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.506 Why?  
RESPONSE: The data come from high-pressure studies and are 
limited by the DAC opening angle.
;
_vrf_PLAT342_impbbr3_235gpa      
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............      0.105 Ang.  
RESPONSE: Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the X-ray 
radiation to the measured sample; poor quality of measurement
;
_vrf_PLAT090_impbbr3_235gpa      
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       4.41 Note  
RESPONSE: The data/parameter ratio is affected by the access limits of the DAC.
;
_vrf_PLAT911_impbbr3_235gpa      
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        344 Report
RESPONSE: These reflections were probably affected 
by unexpected deviations in their intensities for symmetry 
equivalent measurements and omitted during initial data reduction.
;
_vrf_PLAT987_impbbr3_235gpa      
;
PROBLEM: The Flack x is >> 0 -  Do a BASF/TWIN Refinement     Please Check 
RESPONSE: The structure was refined as an inversion twin.
;
# end Validation Reply Form
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br3 Pb, C3 H5 N2'
_chemical_formula_sum            'C3 H5 Br3 N2 Pb'
_chemical_formula_weight         516.01
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, z'

_cell_length_a                   13.3713(10)
_cell_length_b                   8.508(4)
_cell_length_c                   14.5938(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1660.3(8)
_cell_formula_units_Z            8
_cell_measurement_pressure       2350000
_cell_measurement_reflns_used    1884
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.3930
_cell_measurement_theta_min      4.7480
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    34.682
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.14374
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
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    4.129
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0884
_diffrn_reflns_av_unetI/netI     0.0720
_diffrn_reflns_Laue_measured_fraction_full 0.506
_diffrn_reflns_Laue_measured_fraction_max 0.356
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7285
_diffrn_reflns_point_group_measured_fraction_full 0.514
_diffrn_reflns_point_group_measured_fraction_max 0.358
_diffrn_reflns_theta_full        15.000
_diffrn_reflns_theta_max         26.720
_diffrn_reflns_theta_min         4.779
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.2413
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.506
_diffrn_measured_fraction_theta_max 0.356
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  19.75   0.75   35.00   0.00 -30.00   0.00    --    73
  2  φ    140.00 200.00   0.75   35.00   0.00 -30.00   0.00    --    80
  3  φ    160.00 217.00   0.75   35.00   0.00  30.00   0.00    --    76
  4  φ    -20.00  34.75   0.75   35.00   0.00  30.00   0.00    --    73
  5  ω    -24.00  24.00   0.75   35.00    --   30.00  39.46 -12.90   64
  6  ω    -24.00  24.00   0.75   35.00    --   30.00  39.46 167.10   64
  7  ω    -50.00  10.00   0.75   35.00    --  -30.00  39.46 167.10   80
  8  ω    -50.00  10.00   0.75   35.00    --  -30.00  39.46 -12.90   80
  9  ω    -64.00  -8.50   0.75   35.00    --  -30.00  81.40 -28.90   74
 10  ω    -64.00  -8.50   0.75   35.00    --  -30.00  81.40 151.10   74
 11  ω    -19.00   8.00   0.75   35.00    --   30.00  81.40 151.10   36
 12  ω    -19.00   8.00   0.75   35.00    --   30.00  81.40 -28.90   36
 13  ω    -43.00 -21.25   0.75   35.00    --   30.00 134.60 -56.90   29
 14  ω    -43.00 -21.25   0.75   35.00    --   30.00 134.60 123.10   29
 15  ω    -90.00 -36.00   0.75   35.00    --  -30.00 134.60 123.10   72
 16  ω    -90.00 -36.00   0.75   35.00    --  -30.00 134.60 -56.90   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.934
_reflns_Friedel_fraction_full    0.524
_reflns_Friedel_fraction_max     0.360
_reflns_number_gt                850
_reflns_number_total             1239
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXD  (Sheldrick, 2008)'
_refine_diff_density_max         0.945
_refine_diff_density_min         -1.018
_refine_diff_density_rms         0.207
_refine_ls_abs_structure_details 
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack   0.5
_refine_ls_extinction_coef       0.00058(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         1239
_refine_ls_number_restraints     189
_refine_ls_R_factor_all          0.0825
_refine_ls_R_factor_gt           0.0443
_refine_ls_restrained_S_all      1.017
_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)+(0.0353P)²+8.6374P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0826
_refine_ls_wR_factor_ref         0.0968
_refine_special_details          
;
 Refined as a 2-component perfect inversion twin.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Rigid bond restraints
 C6, C5, N4, C4, N3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C3, C2, N2, C1, N1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
N3 \\sim C4 \\sim N4 \\sim C5 \\sim C6: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
N2 \\sim C2 \\sim N1 \\sim C1 \\sim C3: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Uanis(N3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(C5) \\sim
Ueq, Uanis(C6) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of
0.008
Uanis(N2) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C1) \\sim
Ueq, Uanis(C3) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of
0.008
Uanis(Br6) \\sim Ueq, Uanis(Br3) \\sim Ueq, Uanis(Pb2) \\sim Ueq, Uanis(Br2)
\\sim Ueq, Uanis(Br5) \\sim Ueq, Uanis(Br4) \\sim Ueq, Uanis(Pb1) \\sim Ueq,
Uanis(Br1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4.a :
 C2(N2,C3,C1,N1), C6(C5,N4,C4,N3)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), N2(H2A), C3(H3), C1(H1), N1(H1A), C6(H6), C5(H5), N4(H4), C4(H4A),
 N3(H3A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.1750(4) 0.0062(9) 0.36838(9) 0.0232(13) Uani 1 1 d . U . . .
Pb2 Pb 0.1754(4) 0.0077(10) 0.62588(9) 0.0243(13) Uani 1 1 d . U . . .
Br1 Br 0.2284(10) 0.283(3) 0.2589(6) 0.031(3) Uani 1 1 d . U . . .
Br2 Br 0.0614(2) 0.2045(10) 0.4952(9) 0.0321(12) Uani 1 1 d . U . . .
Br3 Br 0.0010(14) -0.009(4) 0.7452(9) 0.0292(12) Uani 1 1 d . U . . .
Br4 Br 0.3425(2) 0.0514(10) 0.4881(6) 0.0270(16) Uani 1 1 d . U . . .
Br5 Br 0.1220(2) -0.2566(11) 0.4974(9) 0.0336(12) Uani 1 1 d . U . . .
Br6 Br 0.2259(10) 0.291(3) 0.7362(7) 0.035(3) Uani 1 1 d . U . . .
C2 C 0.2897(17) 0.450(5) 0.484(3) 0.035(9) Uani 1 1 d G U . . .
H2 H 0.248488 0.362789 0.477495 0.042 Uiso 1 1 calc R U . . .
N2 N 0.326(4) 0.535(9) 0.416(3) 0.035(8) Uani 1 1 d G U . . .
H2A H 0.316550 0.519427 0.358375 0.042 Uiso 1 1 calc R U . . .
C3 C 0.381(3) 0.649(7) 0.452(5) 0.029(8) Uani 1 1 d G U . . .
H3 H 0.415663 0.725507 0.419476 0.035 Uiso 1 1 calc R U . . .
C1 C 0.378(3) 0.634(6) 0.542(5) 0.029(8) Uani 1 1 d G U . . .
H1 H 0.410292 0.698295 0.583985 0.035 Uiso 1 1 calc R U . . .
N1 N 0.322(4) 0.511(8) 0.561(3) 0.038(8) Uani 1 1 d G U . . .
H1A H 0.308035 0.476887 0.615433 0.045 Uiso 1 1 calc R U . . .
C6 C 0.497(4) 0.055(10) 0.313(2) 0.037(9) Uani 1 1 d G U . . .
H6 H 0.490914 0.104393 0.369797 0.044 Uiso 1 1 calc R U . . .
C5 C 0.546(3) -0.069(10) 0.295(3) 0.035(9) Uani 1 1 d G U . . .
H5 H 0.583315 -0.127459 0.336934 0.042 Uiso 1 1 calc R U . . .
N4 N 0.535(3) -0.100(8) 0.204(3) 0.033(9) Uani 1 1 d G U . . .
H4 H 0.562288 -0.178957 0.175839 0.039 Uiso 1 1 calc R U . . .
C4 C 0.480(3) 0.003(9) 0.165(2) 0.029(9) Uani 1 1 d G U . . .
H4A H 0.460302 0.009184 0.103728 0.035 Uiso 1 1 calc R U . . .
N3 N 0.456(3) 0.099(9) 0.233(4) 0.039(9) Uani 1 1 d G U . . .
H3A H 0.418499 0.180797 0.226322 0.046 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 2.93(2) . ?
Pb1 Br2 2.929(11) . ?
Pb1 Br3 2.962(17) 2_554 ?
Pb1 Br4 2.866(8) . ?
Pb1 Br5 3.007(13) . ?
Pb1 Br6 2.97(2) 3_544 ?
Pb2 Br1 3.01(2) 3_545 ?
Pb2 Br2 2.960(11) . ?
Pb2 Br3 2.914(17) . ?
Pb2 Br4 3.029(8) . ?
Pb2 Br5 3.014(13) . ?
Pb2 Br6 2.98(2) . ?
C2 H2 0.9300 . ?
C2 N2 1.32(2) . ?
C2 N1 1.32(2) . ?
N2 H2A 0.8600 . ?
N2 C3 1.32(2) . ?
C3 H3 0.9300 . ?
C3 C1 1.32(2) . ?
C1 H1 0.9300 . ?
C1 N1 1.32(2) . ?
N1 H1A 0.8600 . ?
C6 H6 0.9300 . ?
C6 C5 1.27(2) . ?
C6 N3 1.35(3) . ?
C5 H5 0.9300 . ?
C5 N4 1.37(3) . ?
N4 H4 0.8600 . ?
N4 C4 1.29(3) . ?
C4 H4A 0.9300 . ?
C4 N3 1.32(3) . ?
N3 H3A 0.8600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br1 Pb1 Br3 81.7(6) . 2_554 ?
Br1 Pb1 Br5 174.2(4) . . ?
Br1 Pb1 Br6 91.8(8) . 3_544 ?
Br2 Pb1 Br1 90.5(4) . . ?
Br2 Pb1 Br3 88.1(4) . 2_554 ?
Br2 Pb1 Br5 84.9(3) . . ?
Br2 Pb1 Br6 175.1(4) . 3_544 ?
Br3 Pb1 Br5 101.5(5) 2_554 . ?
Br3 Pb1 Br6 88.0(5) 2_554 3_544 ?
Br4 Pb1 Br1 91.9(3) . . ?
Br4 Pb1 Br2 86.7(3) . . ?
Br4 Pb1 Br3 171.8(6) . 2_554 ?
Br4 Pb1 Br5 84.4(3) . . ?
Br4 Pb1 Br6 97.5(3) . 3_544 ?
Br6 Pb1 Br5 93.1(6) 3_544 . ?
Br1 Pb2 Br4 101.0(3) 3_545 . ?
Br1 Pb2 Br5 91.6(5) 3_545 . ?
Br2 Pb2 Br1 173.6(4) . 3_545 ?
Br2 Pb2 Br4 83.3(2) . . ?
Br2 Pb2 Br5 84.2(3) . . ?
Br2 Pb2 Br6 90.4(5) . . ?
Br3 Pb2 Br1 85.8(5) . 3_545 ?
Br3 Pb2 Br2 90.0(4) . . ?
Br3 Pb2 Br4 173.2(5) . . ?
Br3 Pb2 Br5 98.4(5) . . ?
Br3 Pb2 Br6 84.1(6) . . ?
Br5 Pb2 Br4 81.6(2) . . ?
Br6 Pb2 Br1 94.0(8) . 3_545 ?
Br6 Pb2 Br4 95.3(3) . . ?
Br6 Pb2 Br5 174.0(5) . . ?
Pb1 Br1 Pb2 164.6(7) . 3_554 ?
Pb1 Br2 Pb2 79.29(18) . . ?
Pb2 Br3 Pb1 176.7(12) . 2 ?
Pb1 Br4 Pb2 79.14(9) . . ?
Pb1 Br5 Pb2 77.2(2) . . ?
Pb1 Br6 Pb2 162.1(8) 3 . ?
N2 C2 H2 126.0 . . ?
N2 C2 N1 108.0 . . ?
N1 C2 H2 126.0 . . ?
C2 N2 H2A 126.0 . . ?
C2 N2 C3 108.0 . . ?
C3 N2 H2A 126.0 . . ?
N2 C3 H3 126.0 . . ?
N2 C3 C1 108.0 . . ?
C1 C3 H3 126.0 . . ?
C3 C1 H1 126.0 . . ?
N1 C1 C3 108.0 . . ?
N1 C1 H1 126.0 . . ?
C2 N1 H1A 126.0 . . ?
C1 N1 C2 108.0 . . ?
C1 N1 H1A 126.0 . . ?
C5 C6 H6 127.4 . . ?
C5 C6 N3 105.3 . . ?
N3 C6 H6 127.4 . . ?
C6 C5 H5 125.9 . . ?
C6 C5 N4 108.1 . . ?
N4 C5 H5 125.9 . . ?
C5 N4 H4 124.6 . . ?
C4 N4 C5 110.8 . . ?
C4 N4 H4 124.6 . . ?
N4 C4 H4A 128.2 . . ?
N4 C4 N3 103.5 . . ?
N3 C4 H4A 128.2 . . ?
C6 N3 H3A 123.8 . . ?
C4 N3 C6 112.4 . . ?
C4 N3 H3A 123.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 N2 C3 C1 0.0 . . . . ?
N2 C2 N1 C1 0.0 . . . . ?
N2 C3 C1 N1 0.0 . . . . ?
C3 C1 N1 C2 0.0 . . . . ?
N1 C2 N2 C3 0.0 . . . . ?
C6 C5 N4 C4 -0.1 . . . . ?
C5 C6 N3 C4 0.0 . . . . ?
C5 N4 C4 N3 0.0 . . . . ?
N4 C4 N3 C6 0.0 . . . . ?
N3 C6 C5 N4 0.0 . . . . ?

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

data_im2pbbr4_2_84gpa
_database_code_depnum_ccdc_archive 'CCDC 2473973'
loop_
_audit_author_name
_audit_author_address
'Kinga Roszak'
;Adam Mickiewicz University Poznan
Poland
;
_audit_update_record             
;
2025-07-18 deposited with the CCDC.	2026-03-26 downloaded from the CCDC.
;
_audit_creation_date             2023-06-06
# start Validation Reply Form
_vrf_THETM01_im2pbbr4_2_84gpa    
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: Due to the DAC opening angle and low symmetry some of the data can not be collected.
;
_vrf_RINTA01_im2pbbr4_2_84gpa    
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: High factor is a result from the weak diffraction. Due to the specificity 
of the applied measuring technique and use of a diamond-anvil cell 
limiting the access of the X-ray radiation to the measured sample.
;
_vrf_PLAT027_im2pbbr4_2_84gpa    
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      17.50 Degree
RESPONSE: A full set of data was collected, however 
the very high angle data was poor and was omitted.
Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the 
X-ray radiation to the measured sample.
;
_vrf_PLAT029_im2pbbr4_2_84gpa    
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.323 Why?  
RESPONSE: The data come from high-pressure studies and are 
limited by the DAC opening angle.
;
_vrf_PLAT088_im2pbbr4_2_84gpa    
;
PROBLEM: Poor Data / Parameter Ratio ....................       3.53 Note  
RESPONSE: The data/parameter ratio is affected by the access limits of the DAC.
;
_vrf_PLAT020_im2pbbr4_2_84gpa    
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.191 Report
RESPONSE: High factor is a result from the weak diffraction. Due to the specificity 
of the applied measuring technique and use of a diamond-anvil cell 
limiting the access of the X-ray radiation to the measured sample.
;
_vrf_PLAT342_im2pbbr4_2_84gpa    
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............      0.085 Ang.  
RESPONSE: Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the X-ray 
radiation to the measured sample; poor quality of measurement
;
_vrf_PLAT911_im2pbbr4_2_84gpa    
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.528        339 Report
RESPONSE: These reflections were probably affected 
by unexpected deviations in their intensities for symmetry 
equivalent measurements and omitted during initial data reduction.
;
# end Validation Reply Form
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br4 Pb, 2(C3 H5 N2)'
_chemical_formula_sum            'C6 H10 Br4 N4 Pb'
_chemical_formula_weight         665.01
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   5.8316(13)
_cell_length_b                   9.108(3)
_cell_length_c                   12.603(8)
_cell_angle_alpha                72.46(5)
_cell_angle_beta                 83.89(5)
_cell_angle_gamma                86.50(2)
_cell_volume                     634.3(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    439
_cell_measurement_pressure       2840000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18.8000
_cell_measurement_theta_min      3.4440
_shelx_estimated_absorpt_T_max   0.306
_shelx_estimated_absorpt_T_min   0.066
_exptl_absorpt_coefficient_mu    25.870
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6473
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.89a (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_density_diffrn    3.482
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1907
_diffrn_reflns_av_unetI/netI     0.1139
_diffrn_reflns_Laue_measured_fraction_full 0.323
_diffrn_reflns_Laue_measured_fraction_max 0.271
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            4017
_diffrn_reflns_point_group_measured_fraction_full 0.323
_diffrn_reflns_point_group_measured_fraction_max 0.271
_diffrn_reflns_theta_full        17.500
_diffrn_reflns_theta_max         22.061
_diffrn_reflns_theta_min         2.346
_diffrn_ambient_temperature      293(2)
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_detector_area_resol_mean 16.1544
_diffrn_measured_fraction_theta_full 0.323
_diffrn_measured_fraction_theta_max 0.271
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0055448000
_diffrn_orient_matrix_UB_12      0.0112386000
_diffrn_orient_matrix_UB_13      0.0535069000
_diffrn_orient_matrix_UB_21      0.0293570000
_diffrn_orient_matrix_UB_22      -0.0786706000
_diffrn_orient_matrix_UB_23      0.0238546000
_diffrn_orient_matrix_UB_31      0.1186801000
_diffrn_orient_matrix_UB_32      0.0174173000
_diffrn_orient_matrix_UB_33      -0.0090574000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -9.00  22.20   0.80   15.00    --   15.75  39.00 -12.00   39
  2  ω    -26.00  22.00   0.80   15.00    --   15.75  19.00-180.00   60
  3  ω    -20.00  46.40   0.80   15.00    --   15.75 -19.00-180.00   83
  4  ω     -6.00  22.80   0.80   15.00    --   15.75  57.00 150.00   36
  5  ω    -26.00  42.00   0.80   15.00    --   15.75 -26.00   7.00   85
  6  ω    -24.00  -1.60   0.80   15.00    --   15.75  97.00 -35.00   28
  7  ω    -79.00 -23.00   0.80   15.00    --  -16.61 134.00 -56.00   70
  8  ω    -41.00  21.40   0.80   15.00    --  -16.61  39.00 -12.00   78
  9  ω    -23.00   8.20   0.80   15.00    --  -16.61 -39.00-167.00   39
 10  ω    -29.00  38.20   0.80   15.00    --  -16.61 -13.00   3.00   84
 11  ω    -23.00   4.20   0.80   15.00    --  -16.61 -57.00-150.00   34
 12  ω    -79.00 -23.00   0.80   15.00    --  -16.61 134.00 123.00   70
 13  ω    -42.00  25.20   0.80   15.00    --  -16.61  26.00 172.00   84
 14  ω    -16.00  26.40   0.80   15.00    --   15.75  26.00  -7.00   53
 15  ω     -9.00  39.00   0.80   15.00    --   15.75 -67.00  23.00   60
 16  ω     -9.00  40.60   0.80   15.00    --   15.75 -37.00-180.00   62
 17  ω     15.00  44.60   0.80   15.00    --   15.75 -77.00-150.00   37
 18  ω    -42.00  10.00   0.80   15.00    --  -16.61  37.00-180.00   65
 19  ω    -21.00  27.00   0.80   15.00    --  -16.61 -19.00-180.00   60
 20  ω    -26.00  16.40   0.80   15.00    --  -16.61 -26.00-172.00   53
 21  ω    -41.00  11.00   0.80   15.00    --  -16.61  67.00 -23.00   65
 22  ω     22.00  43.60   0.80   15.00    --  -16.61-134.00-123.00   27
 23  ω     22.00  43.60   0.80   15.00    --  -16.61-134.00  56.00   27
 24  ω    -29.00  38.20   0.80   15.00    --   15.75 -13.00   3.00   84
 25  ω    -39.00  29.00   0.80   15.00    --   15.75  13.00 176.00   85
 26  ω    -26.00  42.00   0.80   15.00    --   15.75 -26.00   7.00   85
 27  ω    -18.00  41.20   0.80   15.00    --   15.75 -39.00-167.00   74
 28  ω    -38.00  29.20   0.80   15.00    --   15.75  13.00  -3.00   84
 29  ω    -47.00  21.00   0.80   15.00    --  -16.61  19.00-180.00   85
 30  ω    -39.00  -7.00   0.80   15.00    --  -16.61  13.00  -3.00   40
 31  ω    -34.00  34.00   0.80   15.00    --  -16.61   0.00   0.00   85
 32  ω    -29.00  38.20   0.80   15.00    --  -16.61 -13.00   3.00   84
 33  ω    -34.00  34.00   0.80   15.00    --  -16.61   0.00-180.00   85
;
_diffrn_measurement_method       'ω scans'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                276
_reflns_number_total             424
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.556
_refine_diff_density_min         -0.899
_refine_diff_density_rms         0.228
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         424
_refine_ls_number_restraints     181
_refine_ls_R_factor_all          0.1215
_refine_ls_R_factor_gt           0.0748
_refine_ls_restrained_S_all      0.868
_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)+(0.1236P)²+26.2788P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1811
_refine_ls_wR_factor_ref         0.2142
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 C6-C5
 2.1 with sigma of 0.02
3. Rigid bond restraints
 C6, C4, N3, C5, N4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N2, C2, N1, C1, C3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Br2, Br1, Pb1, Br3, Br4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
N4 \\sim C5 \\sim N3 \\sim C4 \\sim C6: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
C2 \\sim N1 \\sim C1 \\sim C3 \\sim N2: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Br4 \\sim Pb1 \\sim Br3 \\sim Br1 \\sim Br2: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
Uanis(N4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(C6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C2) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C3) \\sim
Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(Br4) \\sim Ueq, Uanis(Br2) \\sim Ueq, Uanis(Pb1) \\sim Ueq, Uanis(Br3)
\\sim Ueq, Uanis(Br1) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
5.a :
 C2(N2,C3,C1,N1), C4(N3,C5,N4,C6)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), N2(H2A), C3(H3), C1(H1), N1(H1A), C4(H4), N3(H3A), C5(H5), N4(H4A),
 C6(H6)
;
_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 0.5334(4) 0.5760(3) 0.3237(7) 0.051(4) Uani 1 1 d . U . . .
Br1 Br 0.4971(11) 0.7285(8) 0.5011(18) 0.052(4) Uani 1 1 d . U . . .
Br2 Br 0.0360(11) 0.5894(8) 0.3406(18) 0.051(5) Uani 1 1 d . U . . .
Br3 Br 0.5180(12) 0.8757(8) 0.1612(19) 0.059(6) Uani 1 1 d . U . . .
Br4 Br 0.5339(12) 0.3993(9) 0.1622(19) 0.057(5) Uani 1 1 d . U . . .
C2 C 1.035(10) 0.663(6) 0.061(10) 0.075(15) Uani 1 1 d G U . . .
H2 H 1.080956 0.576109 0.116758 0.090 Uiso 1 1 calc R U . . .
N2 N 1.137(9) 0.797(6) 0.031(10) 0.076(15) Uani 1 1 d G U . . .
H2A H 1.254222 0.820743 0.057667 0.091 Uiso 1 1 calc R U . . .
C3 C 1.020(10) 0.887(6) -0.049(10) 0.075(15) Uani 1 1 d G U . . .
H3 H 1.051486 0.988969 -0.087066 0.090 Uiso 1 1 calc R U . . .
C1 C 0.846(9) 0.808(6) -0.068(10) 0.065(14) Uani 1 1 d G U . . .
H1 H 0.739359 0.846066 -0.120497 0.079 Uiso 1 1 calc R U . . .
N1 N 0.855(9) 0.669(6) 0.000(10) 0.069(14) Uani 1 1 d G U . . .
H1A H 0.764737 0.595720 0.005595 0.083 Uiso 1 1 calc R U . . .
C4 C 0.047(8) 0.186(4) 0.353(10) 0.043(11) Uani 1 1 d G U . . .
H4 H 0.085311 0.283284 0.354683 0.052 Uiso 1 1 calc R U . . .
N3 N -0.148(7) 0.149(4) 0.331(11) 0.046(11) Uani 1 1 d G U . . .
H3A H -0.266673 0.209302 0.314600 0.055 Uiso 1 1 calc R U . . .
C5 C -0.130(8) 0.000(5) 0.338(10) 0.045(11) Uani 1 1 d DG U . . .
H5 H -0.246886 -0.056959 0.325784 0.053 Uiso 1 1 calc R U . . .
N4 N 0.076(7) -0.056(4) 0.365(10) 0.042(11) Uani 1 1 d G U . . .
H4A H 0.127464 -0.148952 0.373940 0.051 Uiso 1 1 calc R U . . .
C6 C 0.185(7) 0.060(5) 0.374(10) 0.043(11) Uani 1 1 d DG U . . .
H6 H 0.336170 0.054619 0.392503 0.052 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 2.95(2) . ?
Pb1 Br1 2.980(11) 2_666 ?
Pb1 Br2 2.884(7) . ?
Pb1 Br2 2.974(7) 1_655 ?
Pb1 Br3 2.880(11) . ?
Pb1 Br4 2.95(3) . ?
C2 H2 0.9300 . ?
C2 N2 1.32(4) . ?
C2 N1 1.35(4) . ?
N2 H2A 0.8600 . ?
N2 C3 1.32(4) . ?
C3 H3 0.9300 . ?
C3 C1 1.36(4) . ?
C1 H1 0.9300 . ?
C1 N1 1.30(4) . ?
N1 H1A 0.8600 . ?
C4 H4 0.9300 . ?
C4 N3 1.287(13) . ?
C4 C6 1.341(14) . ?
N3 H3A 0.8600 . ?
N3 C5 1.338(14) . ?
C5 H5 0.9300 . ?
C5 N4 1.310(14) . ?
N4 H4A 0.8600 . ?
N4 C6 1.304(14) . ?
C6 H6 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br1 Pb1 Br1 89.3(4) . 2_666 ?
Br1 Pb1 Br2 82.6(5) . 1_655 ?
Br1 Pb1 Br4 173.8(3) . . ?
Br2 Pb1 Br1 91.9(3) 1_655 2_666 ?
Br2 Pb1 Br1 86.7(5) . . ?
Br2 Pb1 Br1 87.6(3) . 2_666 ?
Br2 Pb1 Br2 169.3(9) . 1_655 ?
Br2 Pb1 Br4 89.3(5) . . ?
Br3 Pb1 Br1 88.7(5) . . ?
Br3 Pb1 Br1 174.6(3) . 2_666 ?
Br3 Pb1 Br2 92.8(3) . 1_655 ?
Br3 Pb1 Br2 87.2(2) . . ?
Br3 Pb1 Br4 95.9(6) . . ?
Br4 Pb1 Br1 85.7(5) . 2_666 ?
Br4 Pb1 Br2 101.3(5) . 1_655 ?
Pb1 Br1 Pb1 90.7(4) . 2_666 ?
Pb1 Br2 Pb1 169.3(9) . 1_455 ?
N2 C2 H2 124.7 . . ?
N2 C2 N1 110.5 . . ?
N1 C2 H2 124.7 . . ?
C2 N2 H2A 127.4 . . ?
C3 N2 C2 105.2 . . ?
C3 N2 H2A 127.4 . . ?
N2 C3 H3 125.0 . . ?
N2 C3 C1 110.1 . . ?
C1 C3 H3 125.0 . . ?
C3 C1 H1 126.2 . . ?
N1 C1 C3 107.5 . . ?
N1 C1 H1 126.2 . . ?
C2 N1 H1A 126.6 . . ?
C1 N1 C2 106.7 . . ?
C1 N1 H1A 126.6 . . ?
N3 C4 H4 126.3 . . ?
N3 C4 C6 107.5 . . ?
C6 C4 H4 126.3 . . ?
C4 N3 H3A 126.5 . . ?
C4 N3 C5 107.0 . . ?
C5 N3 H3A 126.5 . . ?
N3 C5 H5 125.0 . . ?
N4 C5 N3 110.1 . . ?
N4 C5 H5 125.0 . . ?
C5 N4 H4A 127.2 . . ?
C6 N4 C5 105.6 . . ?
C6 N4 H4A 127.2 . . ?
C4 C6 H6 125.1 . . ?
N4 C6 C4 109.8 . . ?
N4 C6 H6 125.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 N2 C3 C1 0.0 . . . . ?
N2 C2 N1 C1 0.0 . . . . ?
N2 C3 C1 N1 0.0 . . . . ?
C3 C1 N1 C2 0.0 . . . . ?
N1 C2 N2 C3 0.0 . . . . ?
C4 N3 C5 N4 0.0 . . . . ?
N3 C4 C6 N4 0.0 . . . . ?
N3 C5 N4 C6 0.0 . . . . ?
C5 N4 C6 C4 0.0 . . . . ?
C6 C4 N3 C5 0.0 . . . . ?

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

data_im2pbbr4_3_71gpa
_database_code_depnum_ccdc_archive 'CCDC 2473975'
loop_
_audit_author_name
_audit_author_address
'Kinga Roszak'
;Adam Mickiewicz University Poznan
Poland
;
_audit_update_record             
;
2025-07-18 deposited with the CCDC.	2026-03-26 downloaded from the CCDC.
;
_audit_creation_date             2023-07-04
# start Validation Reply Form
_vrf_PLAT027_im2pbbr4_3_71gpa    
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      17.50 Degree
RESPONSE: A full set of data was collected, however 
the very high angle data was poor and was omitted.
Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the 
X-ray radiation to the measured sample.
;
_vrf_PLAT029_im2pbbr4_3_71gpa    
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.281 Why?  
RESPONSE: The data come from high-pressure studies and are 
limited by the DAC opening angle.
;
_vrf_PLAT088_im2pbbr4_3_71gpa    
;
PROBLEM: Poor Data / Parameter Ratio ....................       3.57 Note  
RESPONSE: The data/parameter ratio is affected by the access limits of the DAC.
;
_vrf_PLAT342_im2pbbr4_3_71gpa    
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............       0.06 Ang.  
RESPONSE: Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the X-ray 
radiation to the measured sample; poor quality of measurement
;
_vrf_PLAT911_im2pbbr4_3_71gpa    
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        359 Report
RESPONSE: These reflections were probably affected 
by unexpected deviations in their intensities for symmetry 
equivalent measurements and omitted during initial data reduction.
;
# end Validation Reply Form
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br4 Pb, 2(C3 H5 N2)'
_chemical_formula_sum            'C6 H10 Br4 N4 Pb'
_chemical_formula_weight         665.01
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   5.7758(5)
_cell_length_b                   9.0820(16)
_cell_length_c                   12.395(6)
_cell_angle_alpha                71.96(3)
_cell_angle_beta                 82.46(2)
_cell_angle_gamma                85.392(10)
_cell_volume                     612.3(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1106
_cell_measurement_pressure       3710000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.3890
_cell_measurement_theta_min      3.5380
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    26.801
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73491
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.89a (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_density_diffrn    3.607
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0644
_diffrn_reflns_av_unetI/netI     0.0580
_diffrn_reflns_Laue_measured_fraction_full 0.281
_diffrn_reflns_Laue_measured_fraction_max 0.149
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       3
_diffrn_reflns_limit_l_min       -3
_diffrn_reflns_number            2353
_diffrn_reflns_point_group_measured_fraction_full 0.281
_diffrn_reflns_point_group_measured_fraction_max 0.149
_diffrn_reflns_theta_full        17.500
_diffrn_reflns_theta_max         27.724
_diffrn_reflns_theta_min         2.361
_diffrn_ambient_temperature      293(2)
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_detector_area_resol_mean 16.1544
_diffrn_measured_fraction_theta_full 0.281
_diffrn_measured_fraction_theta_max 0.149
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0092020000
_diffrn_orient_matrix_UB_12      0.0061526000
_diffrn_orient_matrix_UB_13      0.0560567000
_diffrn_orient_matrix_UB_21      0.0308373000
_diffrn_orient_matrix_UB_22      -0.0798634000
_diffrn_orient_matrix_UB_23      0.0213371000
_diffrn_orient_matrix_UB_31      0.1196680000
_diffrn_orient_matrix_UB_32      0.0174996000
_diffrn_orient_matrix_UB_33      -0.0081914000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      8.00  38.60   0.85   20.00    --   17.79 -57.00-150.00   36
  2  ω     -7.00  16.80   0.85   20.00    --   17.79  39.00 167.00   28
  3  ω      7.00  38.45   0.85   20.00    --   17.79 -57.00  30.00   37
  4  ω    -24.00  16.80   0.85   20.00    --   17.79  19.00-180.00   48
  5  ω    -14.00  20.00   0.85   20.00    --   17.79  26.00  -7.00   40
  6  ω    -39.00  -7.55   0.85   20.00    --  -18.57  57.00 -30.00   37
  7  ω    -39.00  -7.55   0.85   20.00    --  -18.57  57.00 150.00   37
  8  ω    -80.00 -27.30   0.85   20.00    --  -18.57 134.00 123.00   62
  9  ω    -21.00  13.00   0.85   20.00    --  -18.57 -26.00   7.00   40
 10  ω    -16.00  25.65   0.85   20.00    --  -18.57 -19.00-180.00   49
 11  ω    -81.00 -27.45   0.85   20.00    --  -18.57 134.00 -56.00   63
 12  ω    -17.00   2.55   0.85   20.00    --  -18.57 -57.00-150.00   23
 13  ω    -17.00   6.80   0.85   20.00    --  -18.57 -39.00-167.00   28
 14  ω    -17.00   6.80   0.85   20.00    --  -18.57 -39.00  12.00   28
 15  ω    -49.00 -23.50   0.85   20.00    --  -18.57  77.00 -30.00   30
;
_diffrn_measurement_method       'ω scans'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                344
_reflns_number_total             428
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.673
_refine_diff_density_min         -0.600
_refine_diff_density_rms         0.137
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         428
_refine_ls_number_restraints     200
_refine_ls_R_factor_all          0.0695
_refine_ls_R_factor_gt           0.0482
_refine_ls_restrained_S_all      0.875
_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)+(0.0524P)²+15.8951P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1023
_refine_ls_wR_factor_ref         0.1116
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Rigid bond restraints
 N1, N2, C2, C3, C1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C4, N3, C6, C5, N4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C1 \\sim C3 \\sim N2 \\sim C2 \\sim N1: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
C4 \\sim N3 \\sim C5 \\sim N4 \\sim C6: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Uanis(C1) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(N2) \\sim
Ueq, Uanis(C3) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of
0.008
Uanis(N3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C5) \\sim
Ueq, Uanis(N4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
4. Rigid body (RIGU) restrains
 C1, N1, C2, N2, C3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N3, C4, C6, C5, N4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a :
 C2(N2,C3,C1,N1), C4(N3,C5,N4,C6)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), N2(H2A), C3(H3), C1(H1), N1(H1A), C4(H4), N3(H3A), C5(H5), N4(H4A),
 C6(H6)
;
_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 0.5542(2) 0.57615(16) 0.3195(5) 0.073(8) Uani 1 1 d . . . . .
Br1 Br 0.5065(6) 0.7252(4) 0.4974(13) 0.096(19) Uani 1 1 d . . . . .
Br2 Br 0.0594(6) 0.5963(4) 0.3429(12) 0.055(18) Uani 1 1 d . . . . .
Br3 Br 0.5244(7) 0.8830(4) 0.1610(13) 0.074(19) Uani 1 1 d . . . . .
Br4 Br 0.5276(7) 0.3898(4) 0.1568(14) 0.064(19) Uani 1 1 d . . . . .
C2 C 1.026(6) 0.650(3) 0.065(6) 0.059(7) Uani 1 1 d G U . . .
H2 H 1.061698 0.560320 0.123012 0.071 Uiso 1 1 calc R U . . .
N2 N 1.140(5) 0.780(3) 0.038(7) 0.063(7) Uani 1 1 d G U . . .
H2A H 1.255573 0.798176 0.068277 0.076 Uiso 1 1 calc R U . . .
C3 C 1.036(6) 0.875(3) -0.046(7) 0.059(7) Uani 1 1 d G U . . .
H3 H 1.076500 0.976306 -0.083633 0.071 Uiso 1 1 calc R U . . .
C1 C 0.858(6) 0.803(3) -0.070(7) 0.054(7) Uani 1 1 d G U . . .
H1 H 0.759369 0.846701 -0.126142 0.065 Uiso 1 1 calc R U . . .
N1 N 0.852(5) 0.664(3) -0.001(7) 0.051(7) Uani 1 1 d G U . . .
H1A H 0.757369 0.593953 0.001981 0.061 Uiso 1 1 calc R U . . .
C4 C 0.056(5) 0.184(3) 0.353(8) 0.044(8) Uani 1 1 d G U . . .
H4 H 0.090994 0.282534 0.352706 0.053 Uiso 1 1 calc R U . . .
N3 N -0.141(5) 0.144(3) 0.335(8) 0.050(8) Uani 1 1 d G U . . .
H3A H -0.264384 0.202498 0.321785 0.060 Uiso 1 1 calc R U . . .
C5 C -0.119(5) -0.006(3) 0.343(8) 0.046(8) Uani 1 1 d G U . . .
H5 H -0.236050 -0.064101 0.333519 0.055 Uiso 1 1 calc R U . . .
N4 N 0.091(5) -0.057(3) 0.364(7) 0.041(7) Uani 1 1 d G U . . .
H4A H 0.147888 -0.150121 0.372692 0.049 Uiso 1 1 calc R U . . .
C6 C 0.199(5) 0.060(3) 0.370(8) 0.041(8) Uani 1 1 d G U . . .
H6 H 0.353769 0.057144 0.385167 0.049 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br1 2.977(8) 2_666 ?
Pb1 Br1 2.898(17) . ?
Pb1 Br2 2.995(4) 1_655 ?
Pb1 Br2 2.831(4) . ?
Pb1 Br3 2.877(6) . ?
Pb1 Br4 3.031(16) . ?
C2 H2 0.9300 . ?
C2 N2 1.33(2) . ?
C2 N1 1.36(2) . ?
N2 H2A 0.8600 . ?
N2 C3 1.30(2) . ?
C3 H3 0.9300 . ?
C3 C1 1.37(2) . ?
C1 H1 0.9300 . ?
C1 N1 1.29(2) . ?
N1 H1A 0.8600 . ?
C4 H4 0.9300 . ?
C4 N3 1.29(2) . ?
C4 C6 1.32(2) . ?
N3 H3A 0.8600 . ?
N3 C5 1.33(2) . ?
C5 H5 0.9300 . ?
C5 N4 1.30(2) . ?
N4 H4A 0.8600 . ?
N4 C6 1.31(2) . ?
C6 H6 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br1 Pb1 Br1 87.9(2) . 2_666 ?
Br1 Pb1 Br2 94.98(18) 2_666 1_655 ?
Br1 Pb1 Br2 80.2(3) . 1_655 ?
Br1 Pb1 Br4 85.2(3) 2_666 . ?
Br1 Pb1 Br4 169.77(18) . . ?
Br2 Pb1 Br1 84.6(3) . . ?
Br2 Pb1 Br1 84.55(16) . 2_666 ?
Br2 Pb1 Br2 164.8(6) . 1_655 ?
Br2 Pb1 Br3 85.35(14) . . ?
Br2 Pb1 Br4 107.9(3) 1_655 . ?
Br2 Pb1 Br4 87.2(3) . . ?
Br3 Pb1 Br1 86.5(3) . . ?
Br3 Pb1 Br1 168.9(2) . 2_666 ?
Br3 Pb1 Br2 93.53(14) . 1_655 ?
Br3 Pb1 Br4 99.0(4) . . ?
Pb1 Br1 Pb1 92.1(2) . 2_666 ?
Pb1 Br2 Pb1 164.8(6) . 1_455 ?
N2 C2 H2 124.3 . . ?
N2 C2 N1 111.4 . . ?
N1 C2 H2 124.3 . . ?
C2 N2 H2A 127.8 . . ?
C3 N2 C2 104.5 . . ?
C3 N2 H2A 127.8 . . ?
N2 C3 H3 124.9 . . ?
N2 C3 C1 110.3 . . ?
C1 C3 H3 124.9 . . ?
C3 C1 H1 126.1 . . ?
N1 C1 C3 107.8 . . ?
N1 C1 H1 126.1 . . ?
C2 N1 H1A 127.0 . . ?
C1 N1 C2 106.0 . . ?
C1 N1 H1A 127.0 . . ?
N3 C4 H4 126.5 . . ?
N3 C4 C6 107.1 . . ?
C6 C4 H4 126.5 . . ?
C4 N3 H3A 126.1 . . ?
C4 N3 C5 107.8 . . ?
C5 N3 H3A 126.1 . . ?
N3 C5 H5 125.4 . . ?
N4 C5 N3 109.2 . . ?
N4 C5 H5 125.4 . . ?
C5 N4 H4A 126.9 . . ?
C5 N4 C6 106.2 . . ?
C6 N4 H4A 126.9 . . ?
C4 C6 H6 125.2 . . ?
N4 C6 C4 109.7 . . ?
N4 C6 H6 125.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 N2 C3 C1 0.0 . . . . ?
N2 C2 N1 C1 0.0 . . . . ?
N2 C3 C1 N1 0.0 . . . . ?
C3 C1 N1 C2 0.0 . . . . ?
N1 C2 N2 C3 0.0 . . . . ?
C4 N3 C5 N4 0.0 . . . . ?
N3 C4 C6 N4 0.0 . . . . ?
N3 C5 N4 C6 0.0 . . . . ?
C5 N4 C6 C4 0.0 . . . . ?
C6 C4 N3 C5 0.0 . . . . ?

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

data_im2pbbr4_3_26gpa
_database_code_depnum_ccdc_archive 'CCDC 2473974'
loop_
_audit_author_name
_audit_author_address
'Kinga Roszak'
;Adam Mickiewicz University Poznan
Poland
;
_audit_update_record             
;
2025-07-18 deposited with the CCDC.	2026-03-26 downloaded from the CCDC.
;
_audit_creation_date             2023-06-27
# start Validation Reply Form
_vrf_RINTA01_im2pbbr4_3_26gpa    
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: High factor is a result from the weak diffraction. Due to the specificity 
of the applied measuring technique and use of a diamond-anvil cell 
limiting the access of the X-ray radiation to the measured sample.
;
_vrf_PLAT027_im2pbbr4_3_26gpa    
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      17.50 Degree
RESPONSE: A full set of data was collected, however 
the very high angle data was poor and was omitted.
Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the 
X-ray radiation to the measured sample.
;
_vrf_PLAT029_im2pbbr4_3_26gpa    
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.318 Why?  
RESPONSE: The data come from high-pressure studies and are 
limited by the DAC opening angle.
;
_vrf_PLAT088_im2pbbr4_3_26gpa    
;
PROBLEM: Poor Data / Parameter Ratio ....................       4.50 Note  
RESPONSE: The data/parameter ratio is affected by the access limits of the DAC.
;
_vrf_PLAT342_im2pbbr4_3_26gpa    
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............      0.065 Ang.  
RESPONSE: Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the X-ray 
radiation to the measured sample; poor quality of measurement
;
_vrf_PLAT411_im2pbbr4_3_26gpa    
;
PROBLEM: Short Inter H...H Contact  H3       ..H3       .       1.88 Ang.  
RESPONSE: It is very difficult to locate hydrogen atoms 
accurately using X-ray data because these atoms have low 
scattering power. In addition, we have bad quality measurement 
and low resolution data.
;
_vrf_PLAT911_im2pbbr4_3_26gpa    
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        257 Report
RESPONSE: These reflections were probably affected 
by unexpected deviations in their intensities for symmetry 
equivalent measurements and omitted during initial data reduction.
;
# end Validation Reply Form
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br4 Pb, 2(C3 H5 N2)'
_chemical_formula_sum            'C6 H10 Br4 N4 Pb'
_chemical_formula_weight         665.01
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   5.808(4)
_cell_length_b                   9.096(6)
_cell_length_c                   12.435(15)
_cell_angle_alpha                72.49(10)
_cell_angle_beta                 83.38(10)
_cell_angle_gamma                86.07(5)
_cell_volume                     621.9(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    427
_cell_measurement_pressure       3260000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.1220
_cell_measurement_theta_min      3.4030
_shelx_estimated_absorpt_T_max   0.300
_shelx_estimated_absorpt_T_min   0.064
_exptl_absorpt_coefficient_mu    26.387
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7188
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.89a (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_density_diffrn    3.551
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.2200
_diffrn_reflns_av_unetI/netI     0.2003
_diffrn_reflns_Laue_measured_fraction_full 0.318
_diffrn_reflns_Laue_measured_fraction_max 0.201
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       3
_diffrn_reflns_limit_l_min       -3
_diffrn_reflns_number            4438
_diffrn_reflns_point_group_measured_fraction_full 0.318
_diffrn_reflns_point_group_measured_fraction_max 0.201
_diffrn_reflns_theta_full        17.500
_diffrn_reflns_theta_max         26.821
_diffrn_reflns_theta_min         2.349
_diffrn_ambient_temperature      293(2)
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_detector_area_resol_mean 16.1544
_diffrn_measured_fraction_theta_full 0.318
_diffrn_measured_fraction_theta_max 0.201
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0053404000
_diffrn_orient_matrix_UB_12      0.0082513000
_diffrn_orient_matrix_UB_13      0.0551744000
_diffrn_orient_matrix_UB_21      0.0297762000
_diffrn_orient_matrix_UB_22      -0.0795601000
_diffrn_orient_matrix_UB_23      0.0220044000
_diffrn_orient_matrix_UB_31      0.1192508000
_diffrn_orient_matrix_UB_32      0.0172186000
_diffrn_orient_matrix_UB_33      -0.0091938000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -9.00  22.20   0.80   15.00    --   15.75  39.00 -12.00   39
  2  ω    -26.00  22.00   0.80   15.00    --   15.75  19.00-180.00   60
  3  ω    -20.00  46.40   0.80   15.00    --   15.75 -19.00-180.00   83
  4  ω     -6.00  22.80   0.80   15.00    --   15.75  57.00 150.00   36
  5  ω    -26.00  42.00   0.80   15.00    --   15.75 -26.00   7.00   85
  6  ω    -24.00  -1.60   0.80   15.00    --   15.75  97.00 -35.00   28
  7  ω    -79.00 -23.00   0.80   15.00    --  -16.61 134.00 -56.00   70
  8  ω    -41.00  21.40   0.80   15.00    --  -16.61  39.00 -12.00   78
  9  ω    -23.00   8.20   0.80   15.00    --  -16.61 -39.00-167.00   39
 10  ω    -29.00  38.20   0.80   15.00    --  -16.61 -13.00   3.00   84
 11  ω    -23.00   4.20   0.80   15.00    --  -16.61 -57.00-150.00   34
 12  ω    -79.00 -23.00   0.80   15.00    --  -16.61 134.00 123.00   70
 13  ω    -42.00  25.20   0.80   15.00    --  -16.61  26.00 172.00   84
 14  ω    -16.00  26.40   0.80   15.00    --   15.75  26.00  -7.00   53
 15  ω     -9.00  39.00   0.80   15.00    --   15.75 -67.00  23.00   60
 16  ω     -9.00  40.60   0.80   15.00    --   15.75 -37.00-180.00   62
 17  ω     15.00  44.60   0.80   15.00    --   15.75 -77.00-150.00   37
 18  ω    -42.00  10.00   0.80   15.00    --  -16.61  37.00-180.00   65
 19  ω    -21.00  27.00   0.80   15.00    --  -16.61 -19.00-180.00   60
 20  ω    -26.00  16.40   0.80   15.00    --  -16.61 -26.00-172.00   53
 21  ω    -41.00  11.00   0.80   15.00    --  -16.61  67.00 -23.00   65
 22  ω     22.00  43.60   0.80   15.00    --  -16.61-134.00-123.00   27
 23  ω     22.00  43.60   0.80   15.00    --  -16.61-134.00  56.00   27
 24  ω    -29.00  38.20   0.80   15.00    --   15.75 -13.00   3.00   84
 25  ω    -39.00  29.00   0.80   15.00    --   15.75  13.00 176.00   85
 26  ω    -26.00  42.00   0.80   15.00    --   15.75 -26.00   7.00   85
 27  ω    -18.00  41.20   0.80   15.00    --   15.75 -39.00-167.00   74
 28  ω    -38.00  29.20   0.80   15.00    --   15.75  13.00  -3.00   84
 29  ω    -47.00  21.00   0.80   15.00    --  -16.61  19.00-180.00   85
 30  ω    -39.00  -7.00   0.80   15.00    --  -16.61  13.00  -3.00   40
 31  ω    -34.00  34.00   0.80   15.00    --  -16.61   0.00   0.00   85
 32  ω    -29.00  38.20   0.80   15.00    --  -16.61 -13.00   3.00   84
 33  ω    -34.00  34.00   0.80   15.00    --  -16.61   0.00-180.00   85
;
_diffrn_measurement_method       'ω scans'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                275
_reflns_number_total             540
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.848
_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.186
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         540
_refine_ls_number_restraints     185
_refine_ls_R_factor_all          0.1649
_refine_ls_R_factor_gt           0.0640
_refine_ls_restrained_S_all      0.894
_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)+(0.0681P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1199
_refine_ls_wR_factor_ref         0.1616
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 N1-C1
 1.27 with sigma of 0.02
 C3-C2
 2.2 with sigma of 0.02
 N2-C3
 1.27 with sigma of 0.02
 N2-C2
 1.27 with sigma of 0.02
 C6-C5
 2.2 with sigma of 0.02
3. Rigid bond restraints
 C5, N4, C6, C4, N3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N1, C1, C3, N2, C2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N1, C2, N2, C3, C1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Pb1, Br1, Br2, Br3, Br4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
N4 \\sim C6 \\sim C4 \\sim N3 \\sim C5: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
C2 \\sim N2 \\sim C3 \\sim C1 \\sim N1: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Br1 \\sim Pb1 \\sim Br3 \\sim Br4 \\sim Br2: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
Uanis(N4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(C6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C2) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C1) \\sim
Ueq, Uanis(N1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(Br1) \\sim Ueq, Uanis(Pb1) \\sim Ueq, Uanis(Br2) \\sim Ueq, Uanis(Br3)
\\sim Ueq, Uanis(Br4) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
5.a :
 C2(N2,C3,C1,N1), C4(N3,C5,N4,C6)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), N2(H2A), C3(H3), C1(H1), N1(H1A), C4(H4), N3(H3A), C5(H5), N4(H4A),
 C6(H6)
;
_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 0.5422(3) 0.5762(2) 0.3229(6) 0.048(3) Uani 1 1 d . U . . .
Br1 Br 0.5018(9) 0.7280(6) 0.4975(14) 0.048(3) Uani 1 1 d . U . . .
Br2 Br 0.0459(8) 0.5915(6) 0.3381(14) 0.048(4) Uani 1 1 d . U . . .
Br3 Br 0.5209(9) 0.8779(6) 0.1618(15) 0.056(5) Uani 1 1 d . U . . .
Br4 Br 0.5330(9) 0.3964(6) 0.1599(15) 0.052(4) Uani 1 1 d . U . . .
C2 C 1.053(7) 0.661(4) 0.064(7) 0.070(12) Uani 1 1 d DG U . . .
H2 H 1.109954 0.573598 0.116604 0.084 Uiso 1 1 calc R U . . .
N2 N 1.142(6) 0.801(4) 0.037(8) 0.073(12) Uani 1 1 d DG U . . .
H2A H 1.257738 0.826720 0.063227 0.088 Uiso 1 1 calc R U . . .
C3 C 1.012(7) 0.889(3) -0.039(8) 0.068(12) Uani 1 1 d DG U . . .
H3 H 1.032104 0.994237 -0.074370 0.081 Uiso 1 1 calc R U . . .
C1 C 0.844(6) 0.805(5) -0.059(7) 0.060(12) Uani 1 1 d DG U . . .
H1 H 0.731777 0.841829 -0.109090 0.072 Uiso 1 1 calc R U . . .
N1 N 0.869(6) 0.663(4) 0.005(7) 0.063(12) Uani 1 1 d DG U . . .
H1A H 0.786432 0.586847 0.009190 0.076 Uiso 1 1 calc R U . . .
C4 C 0.057(6) 0.198(3) 0.345(8) 0.038(10) Uani 1 1 d G U . . .
H4 H 0.093632 0.298974 0.336003 0.045 Uiso 1 1 calc R U . . .
N3 N -0.132(5) 0.152(3) 0.315(7) 0.037(9) Uani 1 1 d G U . . .
H3A H -0.243938 0.211102 0.284016 0.044 Uiso 1 1 calc R U . . .
C5 C -0.117(6) -0.007(3) 0.343(7) 0.041(10) Uani 1 1 d DG U . . .
H5 H -0.227441 -0.068152 0.331138 0.049 Uiso 1 1 calc R U . . .
N4 N 0.082(5) -0.060(3) 0.390(7) 0.034(9) Uani 1 1 d G U . . .
H4A H 0.130022 -0.154207 0.414277 0.041 Uiso 1 1 calc R U . . .
C6 C 0.189(6) 0.067(3) 0.391(7) 0.036(10) Uani 1 1 d DG U . . .
H6 H 0.331473 0.065827 0.419071 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 Br1 2.885(19) . ?
Pb1 Br1 2.993(9) 2_666 ?
Pb1 Br2 2.864(5) . ?
Pb1 Br2 2.968(6) 1_655 ?
Pb1 Br3 2.874(9) . ?
Pb1 Br4 2.970(19) . ?
C2 H2 0.9300 . ?
C2 N2 1.335(9) . ?
C2 N1 1.360(9) . ?
N2 H2A 0.8600 . ?
N2 C3 1.317(9) . ?
C3 H3 0.9300 . ?
C3 C1 1.371(9) . ?
C1 H1 0.9300 . ?
C1 N1 1.302(9) . ?
N1 H1A 0.8600 . ?
C4 H4 0.9300 . ?
C4 N3 1.330(12) . ?
C4 C6 1.380(12) . ?
N3 H3A 0.8600 . ?
N3 C5 1.382(12) . ?
C5 H5 0.9300 . ?
C5 N4 1.348(12) . ?
N4 H4A 0.8600 . ?
N4 C6 1.351(12) . ?
C6 H6 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br1 Pb1 Br1 89.3(3) . 2_666 ?
Br1 Pb1 Br2 82.7(4) . 1_655 ?
Br1 Pb1 Br4 172.7(3) . . ?
Br2 Pb1 Br1 86.9(4) . . ?
Br2 Pb1 Br1 86.6(2) . 2_666 ?
Br2 Pb1 Br1 93.8(2) 1_655 2_666 ?
Br2 Pb1 Br2 169.6(7) . 1_655 ?
Br2 Pb1 Br3 86.2(2) . . ?
Br2 Pb1 Br4 102.8(4) 1_655 . ?
Br2 Pb1 Br4 87.6(4) . . ?
Br3 Pb1 Br1 87.3(4) . . ?
Br3 Pb1 Br1 172.2(3) . 2_666 ?
Br3 Pb1 Br2 92.8(2) . 1_655 ?
Br3 Pb1 Br4 97.2(5) . . ?
Br4 Pb1 Br1 85.6(4) . 2_666 ?
Pb1 Br1 Pb1 90.7(3) . 2_666 ?
Pb1 Br2 Pb1 169.6(7) . 1_455 ?
N2 C2 H2 124.6 . . ?
N2 C2 N1 110.8 . . ?
N1 C2 H2 124.6 . . ?
C2 N2 H2A 127.5 . . ?
C3 N2 C2 104(5) . . ?
C3 N2 H2A 127.5 . . ?
N2 C3 H3 125.0 . . ?
N2 C3 C1 111(5) . . ?
C1 C3 H3 125.0 . . ?
C3 C1 H1 126.1 . . ?
N1 C1 C3 107.8 . . ?
N1 C1 H1 126.1 . . ?
C2 N1 H1A 126.8 . . ?
C1 N1 C2 106.4 . . ?
C1 N1 H1A 126.8 . . ?
N3 C4 H4 126.4 . . ?
N3 C4 C6 107.2 . . ?
C6 C4 H4 126.4 . . ?
C4 N3 H3A 126.3 . . ?
C4 N3 C5 107.4 . . ?
C5 N3 H3A 126.3 . . ?
N3 C5 H5 125.1 . . ?
N4 C5 N3 109.9 . . ?
N4 C5 H5 125.1 . . ?
C5 N4 H4A 127.2 . . ?
C5 N4 C6 105.6 . . ?
C6 N4 H4A 127.2 . . ?
C4 C6 H6 125.0 . . ?
N4 C6 C4 109.9 . . ?
N4 C6 H6 125.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 N2 C3 C1 0.0 . . . . ?
N2 C2 N1 C1 0.0 . . . . ?
N2 C3 C1 N1 0.0 . . . . ?
C3 C1 N1 C2 0.0 . . . . ?
N1 C2 N2 C3 0.0 . . . . ?
C4 N3 C5 N4 0.0 . . . . ?
N3 C4 C6 N4 0.0 . . . . ?
N3 C5 N4 C6 0.0 . . . . ?
C5 N4 C6 C4 0.0 . . . . ?
C6 C4 N3 C5 0.0 . . . . ?

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

data_im2pbbr4_1_80gpa
_database_code_depnum_ccdc_archive 'CCDC 2473971'
loop_
_audit_author_name
_audit_author_address
'Kinga Roszak'
;Adam Mickiewicz University Poznan
Poland
;
_audit_update_record             
;
2025-07-18 deposited with the CCDC.	2026-03-26 downloaded from the CCDC.
;
_audit_creation_date             2024-08-19
# start Validation Reply Form
_vrf_PLAT027_im2pbbr4_1_80gpa    
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      17.50 Degree
RESPONSE: A full set of data was collected, however 
the very high angle data was poor and was omitted.
Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the 
X-ray radiation to the measured sample.
;
_vrf_PLAT029_im2pbbr4_1_80gpa    
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.314 Why?  
RESPONSE: The data come from high-pressure studies and are 
limited by the DAC opening angle.
;
_vrf_PLAT088_im2pbbr4_1_80gpa    
;
PROBLEM: Poor Data / Parameter Ratio ....................       5.28 Note  
RESPONSE: The data/parameter ratio is affected by the access limits of the DAC.
;
_vrf_PLAT342_im2pbbr4_1_80gpa    
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............       0.05 Ang.  
RESPONSE: Due to the specificity of the applied measuring technique 
and use of a diamond-anvil cell limiting the access of the X-ray 
radiation to the measured sample; poor quality of measurement
;
_vrf_PLAT911_im2pbbr4_1_80gpa    
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        452 Report
RESPONSE: These reflections were probably affected 
by unexpected deviations in their intensities for symmetry 
equivalent measurements and omitted during initial data reduction.
;
# end Validation Reply Form
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br4 Pb, 2(C3 H5 N2)'
_chemical_formula_sum            'C6 H10 Br4 N4 Pb'
_chemical_formula_weight         665.01
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   5.9111(6)
_cell_length_b                   9.1347(17)
_cell_length_c                   12.854(5)
_cell_angle_alpha                73.64(3)
_cell_angle_beta                 84.56(2)
_cell_angle_gamma                87.363(13)
_cell_volume                     662.8(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1063
_cell_measurement_temperature    293(2)
_cell_measurement_pressure       1800000
_cell_measurement_theta_max      22.7600
_cell_measurement_theta_min      3.4010
_shelx_estimated_absorpt_T_max   0.318
_shelx_estimated_absorpt_T_min   0.070
_exptl_absorpt_coefficient_mu    24.759
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6205
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.89a (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    3.332
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1492
_diffrn_reflns_av_unetI/netI     0.0947
_diffrn_reflns_Laue_measured_fraction_full 0.314
_diffrn_reflns_Laue_measured_fraction_max 0.184
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            6104
_diffrn_reflns_point_group_measured_fraction_full 0.314
_diffrn_reflns_point_group_measured_fraction_max 0.184
_diffrn_reflns_theta_full        17.500
_diffrn_reflns_theta_max         28.791
_diffrn_reflns_theta_min         2.324
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.1544
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.314
_diffrn_measured_fraction_theta_max 0.184
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -14.00  30.00   0.80   20.00    --   17.79  26.00  -7.00   55
  2  ω    -16.00  41.60   0.80   20.00    --   17.79 -67.00  23.00   72
  3  ω     30.00  58.00   0.80   20.00    --   17.79 -99.00  60.00   35
  4  ω    -26.00  26.00   0.80   20.00    --   17.79  19.00-180.00   65
  5  ω     -4.00  28.00   0.80   20.00    --   17.79  57.00 150.00   40
  6  ω     30.00  58.00   0.80   20.00    --   17.79 -99.00-120.00   35
  7  ω     -4.00  38.40   0.80   20.00    --   17.79 -57.00-150.00   53
  8  ω    -81.00 -17.00   0.80   20.00    --  -18.57 134.00 -56.00   80
  9  ω    -44.00  26.40   0.80   20.00    --  -18.57  39.00 167.00   88
 10  ω    -81.00 -17.00   0.80   20.00    --  -18.57 134.00 123.00   80
 11  ω     17.00  42.60   0.80   20.00    --  -18.57-134.00  56.00   32
 12  ω    -52.00  -4.00   0.80   20.00    --  -18.57  19.00-150.00   60
 13  ω     17.00  42.60   0.80   20.00    --  -18.57-134.00-123.00   32
 14  ω    -39.00  38.60   0.80   20.00    --  -18.57   0.00   0.00   97
 15  ω      5.00  29.00   0.80   20.00    --  -18.57-114.00-136.00   30
 16  ω    -31.00  13.00   0.80   20.00    --  -18.57 -26.00-172.00   55
 17  ω    -44.00 -17.60   0.80   20.00    --   17.79 134.00 -56.00   33
 18  ω     -3.20  44.00   0.80   20.00    --   17.79  57.00 -60.00   59
 19  ω     -9.00  35.00   0.80   20.00    --   17.79 -81.00  29.00   55
 20  ω    -14.00  30.00   0.80   20.00    --   17.79  26.00 172.00   55
 21  ω    -51.00  10.60   0.80   20.00    --  -18.57  81.00 -29.00   77
 22  ω    -43.00  17.00   0.80   20.00    --  -18.57  67.00 157.00   75
 23  ω    -28.00   2.40   0.80   20.00    --  -18.57 -57.00  30.00   38
 24  ω    -31.00  13.00   0.80   20.00    --  -18.57 -26.00   7.00   55
 25  ω    -17.00   5.40   0.80   20.00    --  -18.57 -67.00-157.00   28
 26  ω    -27.00  25.00   0.80   20.00    --  -18.57 -19.00-180.00   65
 27  ω    -35.00 -15.00   0.80   20.00    --  -18.57  37.00 150.00   25
 28  ω    -35.00 -15.00   0.80   20.00    --  -18.57  37.00   0.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                408
_reflns_number_total             634
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.940
_refine_diff_density_min         -0.809
_refine_diff_density_rms         0.171
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         634
_refine_ls_number_restraints     124
_refine_ls_R_factor_all          0.1109
_refine_ls_R_factor_gt           0.0575
_refine_ls_restrained_S_all      0.948
_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)+(0.0814P)²+0.0943P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1253
_refine_ls_wR_factor_ref         0.1501
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 N1-C2
 1.3 with sigma of 0.02
 N2-C3
 1.3 with sigma of 0.02
3. Rigid bond restraints
 N2, C3, N1, C1, C2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C6, C4, N3, C5, N4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
N1 \\sim C2 \\sim C1 \\sim C3 \\sim N2: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
N4 \\sim C5 \\sim N3 \\sim C4 \\sim C6: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Uanis(C2) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(N1) \\sim
Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5.a :
 C2(N2,C3,C1,N1), C4(N3,C5,N4,C6)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), N2(H2A), C3(H3), C1(H1), N1(H1A), C4(H4), N3(H3A), C5(H5), N4(H4A),
 C6(H6)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.51428(17) 0.57597(14) 0.3270(4) 0.050(5) Uani 1 1 d . . . . .
Br1 Br 0.4959(5) 0.7296(4) 0.5014(10) 0.053(12) Uani 1 1 d . . . . .
Br2 Br 0.0147(5) 0.5749(4) 0.3356(9) 0.050(12) Uani 1 1 d . . . . .
Br3 Br 0.5107(5) 0.8729(4) 0.1685(10) 0.062(12) Uani 1 1 d . . . . .
Br4 Br 0.5332(6) 0.4065(4) 0.1595(10) 0.068(13) Uani 1 1 d . . . . .
C2 C 1.065(5) 0.674(3) 0.038(6) 0.088(10) Uani 1 1 d DG U . . .
H2 H 1.129331 0.592354 0.087438 0.106 Uiso 1 1 calc R U . . .
N2 N 1.146(5) 0.809(4) 0.003(7) 0.087(9) Uani 1 1 d DG U . . .
H2A H 1.268345 0.839477 0.020721 0.105 Uiso 1 1 calc R U . . .
C3 C 1.009(5) 0.888(3) -0.064(7) 0.084(10) Uani 1 1 d DG U . . .
H3 H 1.025227 0.990301 -0.101413 0.100 Uiso 1 1 calc R U . . .
C1 C 0.842(5) 0.803(3) -0.070(6) 0.072(9) Uani 1 1 d G U . . .
H1 H 0.720883 0.833099 -0.112462 0.086 Uiso 1 1 calc R U . . .
N1 N 0.877(5) 0.671(3) -0.007(7) 0.072(9) Uani 1 1 d DG U . . .
H1A H 0.792190 0.592767 0.003854 0.086 Uiso 1 1 calc R U . . .
C4 C 0.063(5) 0.182(3) 0.346(5) 0.056(9) Uani 1 1 d G U . . .
H4 H 0.113106 0.277601 0.344103 0.067 Uiso 1 1 calc R U . . .
N3 N -0.118(4) 0.154(3) 0.305(6) 0.068(9) Uani 1 1 d G U . . .
H3A H -0.212509 0.221309 0.271692 0.082 Uiso 1 1 calc R U . . .
C5 C -0.129(5) 0.004(3) 0.325(6) 0.065(15) Uani 1 1 d G U . . .
H5 H -0.242840 -0.046726 0.304515 0.078 Uiso 1 1 calc R U . . .
N4 N 0.044(4) -0.061(3) 0.378(5) 0.065(17) Uani 1 1 d G U . . .
H4A H 0.073506 -0.157740 0.399607 0.078 Uiso 1 1 calc R U . . .
C6 C 0.162(4) 0.049(3) 0.391(5) 0.061(16) Uani 1 1 d G U . . .
H6 H 0.295490 0.035505 0.425675 0.073 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 2.952(14) . ?
Pb1 Br1 3.030(5) 2_666 ?
Pb1 Br2 2.945(3) . ?
Pb1 Br2 2.970(3) 1_655 ?
Pb1 Br3 2.898(5) . ?
Pb1 Br4 2.977(14) . ?
C2 H2 0.9300 . ?
C2 N2 1.281(12) . ?
C2 N1 1.304(12) . ?
N2 H2A 0.8600 . ?
N2 C3 1.281(12) . ?
C3 H3 0.9300 . ?
C3 C1 1.304(12) . ?
C1 H1 0.9300 . ?
C1 N1 1.268(12) . ?
N1 H1A 0.8600 . ?
C4 H4 0.9300 . ?
C4 N3 1.294(19) . ?
C4 C6 1.33(2) . ?
N3 H3A 0.8600 . ?
N3 C5 1.33(2) . ?
C5 H5 0.9300 . ?
C5 N4 1.31(2) . ?
N4 H4A 0.8600 . ?
N4 C6 1.31(2) . ?
C6 H6 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br1 Pb1 Br1 89.3(2) . 2_666 ?
Br1 Pb1 Br2 85.0(2) . 1_655 ?
Br1 Pb1 Br4 177.22(18) . . ?
Br2 Pb1 Br1 91.5(2) . . ?
Br2 Pb1 Br1 88.49(12) 1_655 2_666 ?
Br2 Pb1 Br1 89.24(13) . 2_666 ?
Br2 Pb1 Br2 175.8(5) . 1_655 ?
Br2 Pb1 Br4 88.6(2) . . ?
Br2 Pb1 Br4 94.8(2) 1_655 . ?
Br3 Pb1 Br1 89.0(3) . . ?
Br3 Pb1 Br1 177.7(3) . 2_666 ?
Br3 Pb1 Br2 89.31(12) . . ?
Br3 Pb1 Br2 92.85(12) . 1_655 ?
Br3 Pb1 Br4 93.8(3) . . ?
Br4 Pb1 Br1 88.0(3) . 2_666 ?
Pb1 Br1 Pb1 90.7(2) . 2_666 ?
Pb1 Br2 Pb1 175.8(5) . 1_455 ?
N2 C2 H2 125.3 . . ?
N2 C2 N1 109.4 . . ?
N1 C2 H2 125.3 . . ?
C2 N2 H2A 126.9 . . ?
C2 N2 C3 106.2 . . ?
C3 N2 H2A 126.9 . . ?
N2 C3 H3 125.3 . . ?
N2 C3 C1 109.5 . . ?
C1 C3 H3 125.3 . . ?
C3 C1 H1 126.3 . . ?
N1 C1 C3 107.4 . . ?
N1 C1 H1 126.3 . . ?
C2 N1 H1A 126.3 . . ?
C1 N1 C2 107.5 . . ?
C1 N1 H1A 126.3 . . ?
N3 C4 H4 126.2 . . ?
N3 C4 C6 107.5 . . ?
C6 C4 H4 126.2 . . ?
C4 N3 H3A 126.3 . . ?
C4 N3 C5 107.5 . . ?
C5 N3 H3A 126.3 . . ?
N3 C5 H5 125.3 . . ?
N4 C5 N3 109.3 . . ?
N4 C5 H5 125.3 . . ?
C5 N4 H4A 126.8 . . ?
C6 N4 C5 106.4 . . ?
C6 N4 H4A 126.8 . . ?
C4 C6 H6 125.4 . . ?
N4 C6 C4 109.3 . . ?
N4 C6 H6 125.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 N2 C3 C1 0.0 . . . . ?
N2 C2 N1 C1 0.1 . . . . ?
N2 C3 C1 N1 0.0 . . . . ?
C3 C1 N1 C2 0.0 . . . . ?
N1 C2 N2 C3 0.0 . . . . ?
C4 N3 C5 N4 0.0 . . . . ?
N3 C4 C6 N4 0.0 . . . . ?
N3 C5 N4 C6 0.0 . . . . ?
C5 N4 C6 C4 0.0 . . . . ?
C6 C4 N3 C5 0.0 . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
