# Supplementary Information (SI) for Chemical Science.
# 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_3ClPr2PbBr4_295K
_database_code_depnum_ccdc_archive 'CCDC 2336099'
loop_
_audit_author_name
_audit_author_address
'Dawid Drozdowski'
;Institute of Low Temperature and Structure Research Polish Academy of Sciences
Poland
;
_audit_update_record             
;
2024-02-28 deposited with the CCDC.	2026-06-01 downloaded from the CCDC.
;
_audit_creation_date             2024-02-28
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br4 Pb, 2(C3 H9 Cl N)'
_chemical_formula_sum            'C6 H18 Br4 Cl2 N2 Pb'
_chemical_formula_weight         715.95
_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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           36
_space_group_name_H-M_alt        'C m c 21'
_space_group_name_Hall           'C 2c -2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x, -y, z+1/2'
'-x, y, z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z'

_cell_length_a                   26.852(7)
_cell_length_b                   8.325(3)
_cell_length_c                   8.160(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1824.0(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    19234
_cell_measurement_temperature    295
_cell_measurement_theta_max      29.3300
_cell_measurement_theta_min      2.5500
_shelx_estimated_absorpt_T_max   0.322
_shelx_estimated_absorpt_T_min   0.055
_exptl_absorpt_coefficient_mu    18.284
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.07301
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.93a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.607
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_unetI/netI     0.0160
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            36026
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.348
_diffrn_reflns_theta_min         2.562
_diffrn_ambient_temperature      295
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6249
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -39.00  50.00   1.00   12.00    --   13.47 -77.00 -90.00   89
  2  ω    -18.00  93.00   1.00   12.00    --   13.47  37.00-150.00  111
  3  ω    -23.00  39.00   1.00   12.00    --   13.47  77.00 150.00   62
  4  ω    -39.00  50.00   1.00   12.00    --   13.47 -77.00 150.00   89
  5  ω    -39.00  50.00   1.00   12.00    --   13.47 -77.00  30.00   89
  6  ω    -92.00  18.00   1.00   12.00    --  -14.40 -57.00   0.00  110
  7  ω    -92.00  18.00   1.00   12.00    --  -14.40 -57.00-120.00  110
  8  ω    -44.00  98.00   1.00   12.00    --   13.47  19.00  60.00  142
  9  ω    -23.00  39.00   1.00   12.00    --   13.47  77.00 -60.00   62
 10  ω    -75.00  -3.00   1.00   12.00    --  -14.40 129.00-131.66   72
 11  ω    -87.00 -14.00   1.00   12.00    --  -14.40 146.00  60.32   73
 12  ω    -95.00 -21.00   1.00   12.00    --  -14.40 157.00 140.25   74
 13  ω    -87.00 -14.00   1.00   12.00    --  -14.40 146.00 -34.14   73
 14  ω    -23.00  39.00   1.00   12.00    --   13.47  77.00-150.00   62
 15  ω    -23.00  39.00   1.00   12.00    --   13.47  77.00 120.00   62
 16  ω    -23.00  39.00   1.00   12.00    --   13.47  77.00 -30.00   62
 17  ω    -78.00 105.00   1.00   12.00    --   13.47   0.00-180.00  183
 18  ω    -78.00  59.00   1.00   12.00    --   13.47   0.00-150.00  137
 19  ω    -97.00 -23.00   1.00   12.00    --  -14.40 160.00  16.96   74
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0256669000
_diffrn_orient_matrix_UB_12      -0.0152307000
_diffrn_orient_matrix_UB_13      -0.0135183000
_diffrn_orient_matrix_UB_21      -0.0045987000
_diffrn_orient_matrix_UB_22      0.0838223000
_diffrn_orient_matrix_UB_23      -0.0036987000
_diffrn_orient_matrix_UB_31      0.0042380000
_diffrn_orient_matrix_UB_32      -0.0012078000
_diffrn_orient_matrix_UB_33      -0.0857782000
_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         0.861
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                1754
_reflns_number_total             1908
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (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 (Sheldrick, 2015)'
_refine_diff_density_max         1.095
_refine_diff_density_min         -1.041
_refine_diff_density_rms         0.127
_refine_ls_abs_structure_details 
;
 Flack x determined using 777 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.016(6)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     74
_refine_ls_number_reflns         1908
_refine_ls_number_restraints     22
_refine_ls_R_factor_all          0.0333
_refine_ls_R_factor_gt           0.0277
_refine_ls_restrained_S_all      1.146
_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)+(0.0238P)²+14.4194P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0650
_refine_ls_wR_factor_ref         0.0683
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H) groups
2. Restrained distances
 C3-C2
 1.52 with sigma of 0.01
 C4-C3
 1.52 with sigma of 0.01
 N1-C2
 1.45 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C2 \\sim C3 \\sim C4 \\sim N1: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.03 within 2A
4.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C3(H3A,H3B), C2(H2A,H2B)
4.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_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 0.000000 0.23856(6) 0.10963(10) 0.04408(17) Uani 1 2 d S T P . .
Br2 Br 0.000000 0.55373(19) 0.3037(3) 0.0582(5) Uani 1 2 d S T P . .
Br3 Br 0.11071(6) 0.2697(2) 0.1270(4) 0.0792(6) Uani 1 1 d . . . . .
Br1 Br 0.000000 0.0760(2) 0.4354(3) 0.0863(8) Uani 1 2 d S T P . .
Cl1 Cl 0.2577(2) 0.1486(9) 0.6949(9) 0.146(2) Uani 1 1 d . . . . .
N1 N 0.0971(6) 0.3403(17) 0.5307(16) 0.097(5) Uani 1 1 d D U . . .
H1A H 0.110138 0.356792 0.431930 0.116 Uiso 1 1 calc R U . . .
H1B H 0.100263 0.428839 0.590876 0.116 Uiso 1 1 calc R U . . .
H1C H 0.064935 0.315932 0.520586 0.116 Uiso 1 1 calc R U . . .
C4 C 0.1992(11) 0.107(3) 0.753(4) 0.184(9) Uani 1 1 d D U . . .
H4A H 0.188209 0.001891 0.717781 0.221 Uiso 1 1 calc R U . . .
H4B H 0.194232 0.119482 0.870159 0.221 Uiso 1 1 calc R U . . .
C3 C 0.1752(10) 0.244(3) 0.654(4) 0.194(9) Uani 1 1 d D U . . .
H3A H 0.176456 0.342506 0.717063 0.233 Uiso 1 1 calc R U . . .
H3B H 0.194222 0.260944 0.554033 0.233 Uiso 1 1 calc R U . . .
C2 C 0.1227(11) 0.210(3) 0.610(6) 0.194(9) Uani 1 1 d D U . . .
H2A H 0.122015 0.117079 0.537379 0.233 Uiso 1 1 calc R U . . .
H2B H 0.104731 0.181082 0.708535 0.233 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br2 3.064(2) . ?
Pb1 Br2 3.037(3) 2_564 ?
Pb1 Br3 2.9873(17) . ?
Pb1 Br3 2.9873(17) 4 ?
Pb1 Br1 2.980(2) 2_554 ?
Pb1 Br1 2.983(3) . ?
Cl1 C4 1.68(3) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C2 1.439(13) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C3 1.540(13) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C2 1.481(13) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br2 Pb1 Br2 86.41(3) 2_564 . ?
Br3 Pb1 Br2 89.41(6) 4 2_564 ?
Br3 Pb1 Br2 84.33(4) 4 . ?
Br3 Pb1 Br2 84.33(4) . . ?
Br3 Pb1 Br2 89.41(6) . 2_564 ?
Br3 Pb1 Br3 168.64(7) 4 . ?
Br1 Pb1 Br2 96.21(8) 2_554 2_564 ?
Br1 Pb1 Br2 172.27(7) . 2_564 ?
Br1 Pb1 Br2 85.87(8) . . ?
Br1 Pb1 Br2 177.39(9) 2_554 . ?
Br1 Pb1 Br3 95.68(4) 2_554 4 ?
Br1 Pb1 Br3 89.83(6) . . ?
Br1 Pb1 Br3 89.83(6) . 4 ?
Br1 Pb1 Br3 95.68(4) 2_554 . ?
Br1 Pb1 Br1 91.52(4) 2_554 . ?
Pb1 Br2 Pb1 155.82(8) 2_565 . ?
Pb1 Br1 Pb1 145.48(10) 2 . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C2 N1 H1A 109.5 . . ?
C2 N1 H1B 109.5 . . ?
C2 N1 H1C 109.5 . . ?
Cl1 C4 H4A 112.7 . . ?
Cl1 C4 H4B 112.7 . . ?
H4A C4 H4B 110.2 . . ?
C3 C4 Cl1 95.3(18) . . ?
C3 C4 H4A 112.7 . . ?
C3 C4 H4B 112.7 . . ?
C4 C3 H3A 109.1 . . ?
C4 C3 H3B 109.1 . . ?
H3A C3 H3B 107.8 . . ?
C2 C3 C4 112(2) . . ?
C2 C3 H3A 109.1 . . ?
C2 C3 H3B 109.1 . . ?
N1 C2 C3 115(2) . . ?
N1 C2 H2A 108.6 . . ?
N1 C2 H2B 108.6 . . ?
C3 C2 H2A 108.6 . . ?
C3 C2 H2B 108.6 . . ?
H2A C2 H2B 107.6 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1A Br3 0.89 2.59 3.366(14) 146.0 . yes
N1 H1B Br3 0.89 2.54 3.361(15) 153.2 3_565 yes
N1 H1C Br1 0.89 2.74 3.498(17) 143.7 . yes

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
Cl1 C4 C3 C2 154(3) . . . . ?
C4 C3 C2 N1 174(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 7.361
_oxdiff_exptl_absorpt_empirical_full_min 0.490
####################################################################### 
# 
# 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_3ClPr2PbBr4_370K
_database_code_depnum_ccdc_archive 'CCDC 2336098'
loop_
_audit_author_name
_audit_author_address
'Dawid Drozdowski'
;Institute of Low Temperature and Structure Research Polish Academy of Sciences
Poland
;
_audit_update_record             
;
2024-02-28 deposited with the CCDC.	2026-06-01 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT242_3ClPr2PbBr4_370K    
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        Pb1 Check
RESPONSE: High thermal dynamics of chlorines.
;
# Added during the CSD deposition process: Wednesday 28 February 2024 05:25 PM
# end Validation Reply Form

_audit_creation_date             2024-02-28
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br4 Pb, C4 Cl2, 2(C), N2'
_chemical_formula_sum            'C6 Br4 Cl2 N2 Pb'
_chemical_formula_weight         697.81
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           64
_space_group_name_H-M_alt        'C m c e'
_space_group_name_Hall           '-C 2bc 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y+1/2, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y-1/2, -z-1/2'
'x, -y-1/2, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y, -z-1/2'
'x+1/2, -y, z-1/2'
'-x+1/2, y+1/2, z'

_cell_length_a                   27.554(7)
_cell_length_b                   8.280(3)
_cell_length_c                   8.283(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1889.7(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1539
_cell_measurement_temperature    370.01(10)
_cell_measurement_theta_max      23.4830
_cell_measurement_theta_min      3.5140
_shelx_estimated_absorpt_T_max   0.333
_shelx_estimated_absorpt_T_min   0.057
_exptl_absorpt_coefficient_mu    17.646
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.11396
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.93a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.453
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0552
_diffrn_reflns_av_unetI/netI     0.0475
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4561
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.332
_diffrn_reflns_theta_min         2.957
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      370.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6249
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -64.00  46.00   1.00   12.00    --   13.47 -57.00   0.00  110
  2  ω    -23.00  39.00   1.00   12.00    --   13.47  77.00 120.00   62
  3  ω    -50.00   5.00   1.00   12.00    --  -14.40  77.00-180.00   55
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0183057000
_diffrn_orient_matrix_UB_12      0.0589993000
_diffrn_orient_matrix_UB_13      -0.0121249000
_diffrn_orient_matrix_UB_21      0.0177152000
_diffrn_orient_matrix_UB_22      -0.0619670000
_diffrn_orient_matrix_UB_23      -0.0048490000
_diffrn_orient_matrix_UB_31      -0.0036601000
_diffrn_orient_matrix_UB_32      -0.0049024000
_diffrn_orient_matrix_UB_33      -0.0846183000
_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         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                579
_reflns_number_total             992
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (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 (Sheldrick, 2015)'
_refine_diff_density_max         1.766
_refine_diff_density_min         -0.906
_refine_diff_density_rms         0.158
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     57
_refine_ls_number_reflns         992
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.0881
_refine_ls_R_factor_gt           0.0446
_refine_ls_restrained_S_all      0.994
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0597P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1016
_refine_ls_wR_factor_ref         0.1258
_refine_special_details          ?
_olex2_refinement_description    
;
1. Uiso/Uaniso restraints and constraints
N5 \\sim C4 \\sim C3 \\sim C2: within 2A with sigma of 0.02 and sigma for
terminal atoms of 0.04 within 2A
Uanis(Cl1) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(Cl1) = Uanis(Cl1)
2. Rigid body (RIGU) restrains
 C3, C2, C4, N5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Fixed Sof: Cl1(0.5) N5(0.5) C2(0.5) C3(0.5)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.500000 0.500000 0.500000 0.0750(4) Uani 1 4 d S T P . .
Br2 Br 0.500000 0.1915(2) 0.69150(19) 0.1228(8) Uani 1 2 d S T P . .
Br1 Br 0.39211(10) 0.500000 0.500000 0.1575(11) Uani 1 2 d S T P . .
Cl1 Cl 0.2452(14) 0.508(7) 0.418(6) 0.60(4) Uani 0.5 1 d . U P A 2
C4 C 0.110(3) 0.500000 0.500000 0.253(14) Uani 1 2 d S TU P . .
N5 N 0.096(2) 0.412(5) 0.574(6) 0.231(13) Uani 0.5 1 d . U P B 2
C2 C 0.175(3) 0.555(8) 0.440(10) 0.261(15) Uani 0.5 1 d . U P . .
C3 C 0.160(3) 0.439(8) 0.428(9) 0.260(15) Uani 0.5 1 d . U P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br2 3.0068(16) 9_666 ?
Pb1 Br2 3.0073(16) 2_654 ?
Pb1 Br2 3.0073(16) 10_567 ?
Pb1 Br2 3.0068(16) . ?
Pb1 Br1 2.973(3) . ?
Pb1 Br1 2.973(3) 9_666 ?
Cl1 Cl1 1.37(9) 4_566 ?
Cl1 C2 1.98(8) . ?
C4 C4 0.00000(8) 4_566 ?
C4 C2 1.90(11) 4_566 ?
C4 C3 1.57(9) 4_566 ?
N5 N5 1.90(8) 4_566 ?
C2 C2 1.35(13) 4_566 ?
C2 C3 1.17(9) 4_566 ?
C3 C3 1.56(13) 4_566 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br2 Pb1 Br2 180.00(3) 9_666 . ?
Br2 Pb1 Br2 90.02(3) 9_666 10_567 ?
Br2 Pb1 Br2 90.02(3) . 2_654 ?
Br2 Pb1 Br2 180.00(3) 2_654 10_567 ?
Br2 Pb1 Br2 89.98(3) . 10_567 ?
Br2 Pb1 Br2 89.98(3) 9_666 2_654 ?
Br1 Pb1 Br2 90.0 . 10_567 ?
Br1 Pb1 Br2 90.0 9_666 . ?
Br1 Pb1 Br2 90.0 . 2_654 ?
Br1 Pb1 Br2 90.0 . 9_666 ?
Br1 Pb1 Br2 90.0 9_666 9_666 ?
Br1 Pb1 Br2 90.0 . . ?
Br1 Pb1 Br2 90.0 9_666 2_654 ?
Br1 Pb1 Br2 90.0 9_666 10_567 ?
Br1 Pb1 Br1 180.0 9_666 . ?
Pb1 Br2 Pb1 153.66(7) . 2_655 ?
Cl1 Cl1 C2 86(3) 4_566 . ?
C4 C4 C2 0(10) 4_566 4_566 ?
C4 C4 C3 0(10) 4_566 4_566 ?
C3 C4 C2 33(3) 4_566 4_566 ?
C4 N5 N5 23(7) 4_566 4_566 ?
C2 C2 Cl1 86(3) 4_566 . ?
C3 C2 Cl1 116(8) 4_566 . ?
C3 C2 C2 48(5) 4_566 4_566 ?
C2 C3 C3 42(4) 4_566 4_566 ?

_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 4.206
_oxdiff_exptl_absorpt_empirical_full_min 0.403
####################################################################### 
# 
# 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_3ClPr2PbBr4_350K
_database_code_depnum_ccdc_archive 'CCDC 2336101'
loop_
_audit_author_name
_audit_author_address
'Dawid Drozdowski'
;Institute of Low Temperature and Structure Research Polish Academy of Sciences
Poland
;
_audit_update_record             
;
2024-02-28 deposited with the CCDC.	2026-06-01 downloaded from the CCDC.
;
_audit_creation_date             2024-02-28
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br4 Pb, 2(C3 H9 Cl N)'
_chemical_formula_sum            'C6 H18 Br4 Cl2 N2 Pb'
_chemical_formula_weight         715.95
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C6 Br4 Pb1 Cl2 N2'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   26.849(7)
_cell_length_b                   8.335(3)
_cell_length_c                   8.203(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1835.8(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2573
_cell_measurement_temperature    350.00(10)
_cell_measurement_theta_max      26.4510
_cell_measurement_theta_min      2.8710
_shelx_estimated_absorpt_T_max   0.324
_shelx_estimated_absorpt_T_min   0.055
_exptl_absorpt_coefficient_mu    18.167
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.09663
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.93a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.590
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_av_unetI/netI     0.0418
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            9895
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.360
_diffrn_reflns_theta_min         2.876
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      350.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6249
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -18.00  93.00   0.75   12.00    --   13.47  37.00 -60.00  148
  2  ω    -39.00  21.00   0.75   12.00    --  -14.40 -77.00-180.00   80
  3  ω    -68.00  16.00   0.75   12.00    --  -14.40 -57.00  60.00  112
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0188601921
_diffrn_orient_matrix_UB_12      -0.0585237196
_diffrn_orient_matrix_UB_13      0.0119556674
_diffrn_orient_matrix_UB_21      0.0181483819
_diffrn_orient_matrix_UB_22      0.0615952043
_diffrn_orient_matrix_UB_23      0.0048384319
_diffrn_orient_matrix_UB_31      -0.0036797028
_diffrn_orient_matrix_UB_32      0.0047550946
_diffrn_orient_matrix_UB_33      0.0854550709
_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         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1080
_reflns_number_total             1875
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (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 (Sheldrick, 2015)'
_refine_diff_density_max         0.985
_refine_diff_density_min         -0.685
_refine_diff_density_rms         0.157
_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     71
_refine_ls_number_reflns         1875
_refine_ls_number_restraints     20
_refine_ls_R_factor_all          0.1079
_refine_ls_R_factor_gt           0.0595
_refine_ls_restrained_S_all      1.118
_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)+(0.0378P)²+12.3836P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1179
_refine_ls_wR_factor_ref         0.1373
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H) groups
2. Restrained distances
 C2-C3
 1.55 with sigma of 0.01
 C4-C3
 1.55 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C2 \\sim C3 \\sim C4 \\sim N5: within 2A with sigma of 0.02 and sigma for
terminal atoms of 0.04 within 2A
4.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C3(H3A,H3B), C2(H2A,H2B)
4.b Idealised Me refined as rotating group:
 N5(H5A,H5B,H5C)
;
_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 0.500000 0.500000 0.500000 0.0569(3) Uani 1 2 d S . P . .
Br2 Br 0.50293(7) 0.19257(17) 0.69131(17) 0.0922(6) Uani 1 1 d . . . . .
Br1 Br 0.38948(7) 0.4702(2) 0.5155(2) 0.1048(6) Uani 1 1 d . . . . .
Cl1 Cl 0.2537(4) 0.3963(13) 0.5886(15) 0.276(5) Uani 1 1 d . . . . .
N5 N 0.0944(7) 0.577(2) 0.427(2) 0.152(6) Uani 1 1 d . U . . .
H5A H 0.097012 0.544638 0.324514 0.182 Uiso 1 1 calc R U . . .
H5B H 0.109192 0.672036 0.438720 0.182 Uiso 1 1 calc R U . . .
H5C H 0.062314 0.586120 0.453807 0.182 Uiso 1 1 calc R U . . .
C4 C 0.1187(12) 0.458(4) 0.537(4) 0.246(11) Uani 1 1 d D U . . .
H4A H 0.109728 0.349398 0.506519 0.295 Uiso 1 1 calc R U . . .
H4B H 0.109441 0.476154 0.649701 0.295 Uiso 1 1 calc R U . . .
C3 C 0.1747(12) 0.489(4) 0.510(4) 0.267(12) Uani 1 1 d D U . . .
H3A H 0.184553 0.596497 0.540589 0.321 Uiso 1 1 calc R U . . .
H3B H 0.185130 0.465871 0.399358 0.321 Uiso 1 1 calc R U . . .
C2 C 0.1931(13) 0.359(4) 0.635(4) 0.279(13) Uani 1 1 d D U . . .
H2A H 0.182635 0.251267 0.606985 0.334 Uiso 1 1 calc R U . . .
H2B H 0.184673 0.384299 0.746640 0.334 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br2 2.9991(15) 7_565 ?
Pb1 Br2 3.0059(15) . ?
Pb1 Br2 3.0059(15) 5_666 ?
Pb1 Br2 2.9991(15) 3_656 ?
Pb1 Br1 2.981(2) . ?
Pb1 Br1 2.981(2) 5_666 ?
Cl1 C2 1.70(3) . ?
N5 H5A 0.8900 . ?
N5 H5B 0.8900 . ?
N5 H5C 0.8900 . ?
N5 C4 1.49(3) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C3 1.540(10) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C2 1.565(10) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br2 Pb1 Br2 180.00(3) 7_565 3_656 ?
Br2 Pb1 Br2 89.07(3) 3_656 5_666 ?
Br2 Pb1 Br2 90.93(3) 7_565 5_666 ?
Br2 Pb1 Br2 89.07(3) 7_565 . ?
Br2 Pb1 Br2 180.0 5_666 . ?
Br2 Pb1 Br2 90.93(3) 3_656 . ?
Br1 Pb1 Br2 91.00(5) 5_666 3_656 ?
Br1 Pb1 Br2 91.00(5) . 7_565 ?
Br1 Pb1 Br2 86.13(5) . . ?
Br1 Pb1 Br2 89.00(5) . 3_656 ?
Br1 Pb1 Br2 89.00(5) 5_666 7_565 ?
Br1 Pb1 Br2 86.13(5) 5_666 5_666 ?
Br1 Pb1 Br2 93.87(5) . 5_666 ?
Br1 Pb1 Br2 93.87(5) 5_666 . ?
Br1 Pb1 Br1 180.0 5_666 . ?
Pb1 Br2 Pb1 153.69(6) 3_646 . ?
H5A N5 H5B 109.5 . . ?
H5A N5 H5C 109.5 . . ?
H5B N5 H5C 109.5 . . ?
C4 N5 H5A 109.5 . . ?
C4 N5 H5B 109.5 . . ?
C4 N5 H5C 109.5 . . ?
N5 C4 H4A 111.1 . . ?
N5 C4 H4B 111.1 . . ?
N5 C4 C3 103(2) . . ?
H4A C4 H4B 109.0 . . ?
C3 C4 H4A 111.1 . . ?
C3 C4 H4B 111.1 . . ?
C4 C3 H3A 112.6 . . ?
C4 C3 H3B 112.6 . . ?
C4 C3 C2 96(2) . . ?
H3A C3 H3B 110.1 . . ?
C2 C3 H3A 112.6 . . ?
C2 C3 H3B 112.6 . . ?
Cl1 C2 H2A 113.3 . . ?
Cl1 C2 H2B 113.3 . . ?
C3 C2 Cl1 91.9(19) . . ?
C3 C2 H2A 113.3 . . ?
C3 C2 H2B 113.3 . . ?
H2A C2 H2B 110.6 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N5 H5A Br1 0.89 2.56 3.430(17) 164.7 2_564 yes
N5 H5B Br1 0.89 2.56 3.382(17) 153.2 8_665 yes
N5 H5C Br2 0.89 3.06 3.469(18) 110.2 4_456 yes
N5 H5C Br2 0.89 2.77 3.526(17) 144.1 8_665 yes

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
N5 C4 C3 C2 179(2) . . . . ?
C4 C3 C2 Cl1 177(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.848
_oxdiff_exptl_absorpt_empirical_full_min 0.365
####################################################################### 
# 
# 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_3ClPr2PbBr4_100K_mono
_database_code_depnum_ccdc_archive 'CCDC 2336102'
loop_
_audit_author_name
_audit_author_address
'Dawid Drozdowski'
;Institute of Low Temperature and Structure Research Polish Academy of Sciences
Poland
;
_audit_update_record             
;
2024-02-28 deposited with the CCDC.	2026-06-01 downloaded from the CCDC.
;
_audit_creation_date             2024-02-28
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br4 Pb, 2(C3 H9 Cl N)'
_chemical_formula_sum            'C6 H18 Br4 Cl2 N2 Pb'
_chemical_formula_weight         715.95
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C6 N2 Pb Br4 Cl2'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   13.823(4)
_cell_length_b                   7.785(3)
_cell_length_c                   8.504(3)
_cell_angle_alpha                90
_cell_angle_beta                 106.48(3)
_cell_angle_gamma                90
_cell_volume                     877.6(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5196
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      29.0270
_cell_measurement_theta_min      4.7760
_shelx_estimated_absorpt_T_max   0.482
_shelx_estimated_absorpt_T_min   0.088
_exptl_absorpt_coefficient_mu    19.001
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43481
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.93a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.709
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.045
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0528
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            5479
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.675
_diffrn_reflns_theta_min         2.498
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6249
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -64.00  46.00   1.00   12.00    --   13.83 -57.00   0.00  110
  2  ω    -19.00  92.00   1.00   12.00    --   13.83  57.00 -60.00  111
  3  ω    -19.00  92.00   1.00   12.00    --   13.83  57.00-150.00  111
  4  ω    -39.00  21.00   1.00   12.00    --  -14.61 -77.00 -60.00   60
  5  ω    -64.00  46.00   1.00   12.00    --   13.83 -57.00-120.00  110
  6  ω    -22.00  39.00   1.00   12.00    --   13.83  77.00  90.00   61
  7  ω    -20.00  57.00   1.00   12.00    --   13.83 -99.00 150.00   77
  8  ω    -22.00  39.00   1.00   12.00    --   13.83  77.00 150.00   61
  9  ω    -51.00  39.00   1.00   12.00    --  -14.61  77.00-180.00   90
 10  ω   -107.00 -39.00   1.00   12.00    --  -14.61-178.00  60.00   68
 11  ω    -39.00  -6.00   1.00   12.00    --   13.83 -77.00 -60.00   33
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0354875000
_diffrn_orient_matrix_UB_12      0.0671226000
_diffrn_orient_matrix_UB_13      0.0274675000
_diffrn_orient_matrix_UB_21      -0.0399701000
_diffrn_orient_matrix_UB_22      0.0582600000
_diffrn_orient_matrix_UB_23      -0.0032220000
_diffrn_orient_matrix_UB_31      0.0026031000
_diffrn_orient_matrix_UB_32      -0.0201122000
_diffrn_orient_matrix_UB_33      0.0824304000
_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         0.855
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                4342
_reflns_number_total             5479
_reflns_special_details          
;
 _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 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (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  (Sheldrick, 2015)'
_refine_diff_density_max         6.681
_refine_diff_density_min         -1.973
_refine_diff_density_rms         0.399
_refine_ls_abs_structure_details 
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.58(7)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     91
_refine_ls_number_reflns         5479
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0744
_refine_ls_R_factor_gt           0.0599
_refine_ls_restrained_S_all      1.112
_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)+(0.1127P)²+14.7909P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1768
_refine_ls_wR_factor_ref         0.1861
_refine_special_details          'Refined as a 2-component twin.,Twin'
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.590(3)
 0.410(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(Br3) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(Br2) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(Br1) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(C6) = Uanis(Cl2) = Uanis(C8) = Uanis(C7) = Uanis(N5)
Uanis(C4) = Uanis(Cl1) = Uanis(C3) = Uanis(C2) = Uanis(N1)
4.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C4(H4A,H4B), C2(H2A,H2B), C8(H8A,H8B), C3(H3A,H3B)
4.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N5(H5A,H5B,H5C)
;
_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 0.4997(4) 0.5840(8) 0.2528(3) 0.0116(3) Uani 1 1 d . . . . .
Br1 Br 0.5384(8) 0.4060(9) 0.5774(8) 0.023(2) Uani 1 1 d . U . . .
Br2 Br 0.5387(7) 0.2694(8) 0.0738(8) 0.0167(18) Uani 1 1 d . U . . .
Br4 Br 0.2806(8) 0.5262(8) 0.1869(9) 0.0202(19) Uani 1 1 d . . . . .
Br3 Br 0.7199(8) 0.6503(10) 0.3094(9) 0.0209(19) Uani 1 1 d . U . . .
Cl2 Cl -0.0248(16) 0.730(3) 0.5317(19) 0.022(4) Uani 1 1 d . . . . .
Cl1 Cl 1.0263(17) 0.449(2) 0.9669(18) 0.018(4) Uani 1 1 d . . . . .
N1 N 0.695(5) 0.619(8) 0.913(6) 0.018(4) Uani 1 1 d . . . . .
H1A H 0.691837 0.691752 0.828487 0.022 Uiso 1 1 calc R U . . .
H1B H 0.697218 0.680335 1.005197 0.022 Uiso 1 1 calc R U . . .
H1C H 0.640362 0.548909 0.888398 0.022 Uiso 1 1 calc R U . . .
N5 N 0.305(5) 0.559(10) 0.593(6) 0.022(4) Uani 1 1 d . . . . .
H5A H 0.323641 0.562558 0.499126 0.026 Uiso 1 1 calc R U . . .
H5B H 0.294421 0.447850 0.617687 0.026 Uiso 1 1 calc R U . . .
H5C H 0.354173 0.605669 0.676646 0.026 Uiso 1 1 calc R U . . .
C6 C 0.211(6) 0.657(11) 0.571(7) 0.022(4) Uani 1 1 d . . . . .
H6A H 0.223592 0.780682 0.557528 0.026 Uiso 1 1 calc R U . . .
H6B H 0.159557 0.617652 0.470373 0.026 Uiso 1 1 calc R U . . .
C7 C 0.173(5) 0.634(8) 0.709(7) 0.022(4) Uani 1 1 d . . . . .
H7A H 0.228623 0.645872 0.812137 0.026 Uiso 1 1 calc R U . . .
H7B H 0.143006 0.518506 0.706875 0.026 Uiso 1 1 calc R U . . .
C4 C 0.914(6) 0.400(9) 0.800(7) 0.018(4) Uani 1 1 d . . . . .
H4A H 0.931920 0.405501 0.695534 0.022 Uiso 1 1 calc R U . . .
H4B H 0.893601 0.280242 0.813839 0.022 Uiso 1 1 calc R U . . .
C2 C 0.790(6) 0.511(9) 0.944(6) 0.018(4) Uani 1 1 d . . . . .
H2A H 0.775231 0.392200 0.971639 0.022 Uiso 1 1 calc R U . . .
H2B H 0.842787 0.558831 1.037708 0.022 Uiso 1 1 calc R U . . .
C8 C 0.088(6) 0.782(10) 0.699(7) 0.022(4) Uani 1 1 d . . . . .
H8A H 0.114801 0.895456 0.679326 0.026 Uiso 1 1 calc R U . . .
H8B H 0.070647 0.787574 0.804282 0.026 Uiso 1 1 calc R U . . .
C3 C 0.827(5) 0.511(7) 0.786(6) 0.018(4) Uani 1 1 d . . . . .
H3A H 0.771588 0.472506 0.691701 0.022 Uiso 1 1 calc R U . . .
H3B H 0.845524 0.629281 0.764096 0.022 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 3.013(8) 2_656 ?
Pb1 Br1 2.998(8) . ?
Pb1 Br2 3.040(8) 2_655 ?
Pb1 Br2 3.013(8) . ?
Pb1 Br4 2.953(10) . ?
Pb1 Br3 2.989(10) . ?
Cl2 C8 1.83(8) . ?
Cl1 C4 1.82(8) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 H1C 0.9100 . ?
N1 C2 1.51(9) . ?
N5 H5A 0.9100 . ?
N5 H5B 0.9100 . ?
N5 H5C 0.9100 . ?
N5 C6 1.47(9) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 C7 1.43(7) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.63(10) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C3 1.45(11) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.57(6) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br1 Pb1 Br1 87.32(12) . 2_656 ?
Br1 Pb1 Br2 179.2(4) . 2_655 ?
Br1 Pb1 Br2 94.5(3) . . ?
Br1 Pb1 Br2 91.9(3) 2_656 2_655 ?
Br2 Pb1 Br1 178.1(3) . 2_656 ?
Br2 Pb1 Br2 86.23(11) . 2_655 ?
Br4 Pb1 Br1 90.6(3) . . ?
Br4 Pb1 Br1 84.8(3) . 2_656 ?
Br4 Pb1 Br2 89.7(3) . 2_655 ?
Br4 Pb1 Br2 95.8(3) . . ?
Br4 Pb1 Br3 178.1(3) . . ?
Br3 Pb1 Br1 95.0(3) . 2_656 ?
Br3 Pb1 Br1 91.3(3) . . ?
Br3 Pb1 Br2 84.3(3) . . ?
Br3 Pb1 Br2 88.3(3) . 2_655 ?
Pb1 Br1 Pb1 144.7(3) . 2_646 ?
Pb1 Br2 Pb1 146.9(3) . 2_645 ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C2 N1 H1A 109.5 . . ?
C2 N1 H1B 109.5 . . ?
C2 N1 H1C 109.5 . . ?
H5A N5 H5B 109.5 . . ?
H5A N5 H5C 109.5 . . ?
H5B N5 H5C 109.5 . . ?
C6 N5 H5A 109.5 . . ?
C6 N5 H5B 109.5 . . ?
C6 N5 H5C 109.5 . . ?
N5 C6 H6A 109.7 . . ?
N5 C6 H6B 109.7 . . ?
H6A C6 H6B 108.2 . . ?
C7 C6 N5 110(5) . . ?
C7 C6 H6A 109.7 . . ?
C7 C6 H6B 109.7 . . ?
C6 C7 H7A 110.3 . . ?
C6 C7 H7B 110.3 . . ?
C6 C7 C8 107(5) . . ?
H7A C7 H7B 108.6 . . ?
C8 C7 H7A 110.3 . . ?
C8 C7 H7B 110.3 . . ?
Cl1 C4 H4A 108.3 . . ?
Cl1 C4 H4B 108.3 . . ?
H4A C4 H4B 107.4 . . ?
C3 C4 Cl1 116(5) . . ?
C3 C4 H4A 108.3 . . ?
C3 C4 H4B 108.3 . . ?
N1 C2 H2A 109.7 . . ?
N1 C2 H2B 109.7 . . ?
N1 C2 C3 110(5) . . ?
H2A C2 H2B 108.2 . . ?
C3 C2 H2A 109.7 . . ?
C3 C2 H2B 109.7 . . ?
Cl2 C8 H8A 109.9 . . ?
Cl2 C8 H8B 109.9 . . ?
C7 C8 Cl2 109(5) . . ?
C7 C8 H8A 109.9 . . ?
C7 C8 H8B 109.9 . . ?
H8A C8 H8B 108.3 . . ?
C4 C3 C2 114(5) . . ?
C4 C3 H3A 108.9 . . ?
C4 C3 H3B 108.9 . . ?
C2 C3 H3A 108.9 . . ?
C2 C3 H3B 108.9 . . ?
H3A C3 H3B 107.7 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1A Br4 0.91 2.64 3.33(6) 132.8 2_656 yes
N1 H1B Br3 0.91 2.53 3.30(4) 142.6 1_556 yes
N1 H1C Br1 0.91 2.85 3.48(6) 127.7 . yes
N5 H5A Br4 0.91 2.57 3.39(5) 150.0 . yes
N5 H5B Br3 0.91 2.42 3.33(7) 175.9 2_646 yes
N5 H5C Br2 0.91 2.56 3.45(6) 167.6 2_656 yes

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
Cl1 C4 C3 C2 -59(7) . . . . ?
N1 C2 C3 C4 -176(6) . . . . ?
N5 C6 C7 C8 166(6) . . . . ?
C6 C7 C8 Cl2 72(6) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.646
_oxdiff_exptl_absorpt_empirical_full_min 0.640
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.590(3) 3501 15619 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000
0.0000 1.0000
2 0.410(3) 3483 15619 nmt -1.0005 0.0010 -0.9197 -0.0001 -1.0004 -0.0002 0.0006
-0.0001 1.0006

_twin_special_details            
;
Component 2 rotated by -179.9905° 
around [-0.42 0.00 0.91] (reciprocal) or [0.00 -0.00 1.00] (direct)
;
####################################################################### 
# 
# 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_3ClPr2PbBr4_100K
_database_code_depnum_ccdc_archive 'CCDC 2336100'
loop_
_audit_author_name
_audit_author_address
'Dawid Drozdowski'
;Institute of Low Temperature and Structure Research Polish Academy of Sciences
Poland
;
_audit_update_record             
;
2024-03-01 deposited with the CCDC.	2026-06-01 downloaded from the CCDC.
;
_audit_creation_date             2024-03-01
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br4 Pb, 2(C3 H9 Cl N)'
_chemical_formula_sum            'C6 H18 Br4 Cl2 N2 Pb'
_chemical_formula_weight         715.95
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Pb Br4 Cl N C3'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      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                   16.781(5)
_cell_length_b                   26.750(7)
_cell_length_c                   7.907(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3549.4(19)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    7719
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.0580
_cell_measurement_theta_min      3.5950
_shelx_estimated_absorpt_T_max   0.485
_shelx_estimated_absorpt_T_min   0.089
_exptl_absorpt_coefficient_mu    18.792
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.22868
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.93a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.680
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2592
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.045
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0571
_diffrn_reflns_av_unetI/netI     0.0493
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            30729
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         2.544
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6249
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -20.00  57.00   1.00   12.00    --   13.83 -99.00  60.00   77
  2  ω    -18.00  93.00   1.00   12.00    --   13.83  37.00 -30.00  111
  3  ω    -51.00  39.00   1.00   12.00    --  -14.61  77.00 -90.00   90
  4  ω    -22.00  39.00   1.00   12.00    --   13.83  77.00  60.00   61
  5  ω    -93.00 -29.00   1.00   12.00    --  -14.61 -57.00 120.00   64
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0044242000
_diffrn_orient_matrix_UB_12      -0.0176245000
_diffrn_orient_matrix_UB_13      0.0664980000
_diffrn_orient_matrix_UB_21      -0.0091977000
_diffrn_orient_matrix_UB_22      0.0196538000
_diffrn_orient_matrix_UB_23      0.0569147000
_diffrn_orient_matrix_UB_31      -0.0409867000
_diffrn_orient_matrix_UB_32      -0.0024979000
_diffrn_orient_matrix_UB_33      -0.0199142000
_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         0.853
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                5285
_reflns_number_total             6725
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (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  (Sheldrick, 2015)'
_refine_diff_density_max         1.997
_refine_diff_density_min         -1.748
_refine_diff_density_rms         0.199
_refine_ls_abs_structure_details 
;
 Flack x determined using 1924 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.014(7)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         6725
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0397
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0252P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0723
_refine_ls_wR_factor_ref         0.0793
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N13) = Uanis(C14) = Uanis(C15) = Uanis(C16)
3.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C7(H7A,H7B), C10(H10A,H10B), C14(H14A,H14B), C2(H2A,H2B),
 C3(H3A,H3B), C15(H15A,H15B), C6(H6A,H6B), C4(H4A,H4B), C12(H12A,H12B), C8(H8A,
 H8B), C16(H16A,H16B)
3.b Idealised Me refined as rotating group:
 N9(H9A,H9B,H9C), N5(H5A,H5B,H5C), N13(H13A,H13B,H13C), N1(H1A,H1B,H1C)
;
_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 0.50620(3) 0.25805(2) 0.59553(12) 0.01066(14) Uani 1 1 d . . . . .
Pb2 Pb 0.23898(3) 0.24611(2) 1.09629(12) 0.01120(15) Uani 1 1 d . . . . .
Br2 Br 0.34862(9) 0.25014(5) 0.4027(3) 0.0146(4) Uani 1 1 d . . . . .
Br5 Br 0.39682(9) 0.25440(5) 0.9026(2) 0.0141(4) Uani 1 1 d . . . . .
Br6 Br 0.16754(8) 0.23820(6) 0.7538(2) 0.0186(4) Uani 1 1 d . . . . .
Br1 Br 0.57872(8) 0.26495(6) 0.2541(2) 0.0173(4) Uani 1 1 d . . . . .
Br7 Br 0.23995(7) 0.36043(5) 1.0825(3) 0.0164(3) Uani 1 1 d . . . . .
Br3 Br 0.47924(7) 0.36740(5) 0.5832(3) 0.0167(3) Uani 1 1 d . . . . .
Br4 Br 0.50407(6) 0.14512(5) 0.5816(3) 0.0155(3) Uani 1 1 d . . . . .
Br8 Br 0.26682(7) 0.13804(5) 1.0832(3) 0.0182(3) Uani 1 1 d . . . . .
Cl3 Cl 0.5454(2) -0.01638(14) 0.0213(6) 0.0255(11) Uani 1 1 d . . . . .
Cl4 Cl 0.2015(2) -0.00446(15) 0.5368(6) 0.0319(12) Uani 1 1 d . . . . .
Cl2 Cl 0.1947(2) 0.51715(15) 0.4904(6) 0.0285(11) Uani 1 1 d . . . . .
Cl1 Cl 0.5553(2) 0.50301(15) 0.0409(6) 0.0295(12) Uani 1 1 d . . . . .
N9 N 0.4597(6) 0.1635(5) 0.1743(15) 0.018(3) Uani 1 1 d . . . . .
H9A H 0.408284 0.156661 0.146125 0.021 Uiso 1 1 calc R U . . .
H9B H 0.469109 0.196760 0.162037 0.021 Uiso 1 1 calc R U . . .
H9C H 0.468496 0.154427 0.283726 0.021 Uiso 1 1 calc R U . . .
N5 N 0.2868(6) 0.3405(5) 0.6764(15) 0.016(3) Uani 1 1 d . . . . .
H5A H 0.337391 0.350034 0.650482 0.019 Uiso 1 1 calc R U . . .
H5B H 0.281372 0.307084 0.658991 0.019 Uiso 1 1 calc R U . . .
H5C H 0.276550 0.347697 0.786813 0.019 Uiso 1 1 calc R U . . .
N13 N 0.3095(6) 0.1478(5) 0.6633(16) 0.0193(18) Uani 1 1 d . . . . .
H13A H 0.286911 0.175651 0.617964 0.023 Uiso 1 1 calc R U . . .
H13B H 0.363496 0.151002 0.662097 0.023 Uiso 1 1 calc R U . . .
H13C H 0.292486 0.143936 0.771812 0.023 Uiso 1 1 calc R U . . .
N1 N 0.4338(6) 0.3553(5) 0.1677(16) 0.022(4) Uani 1 1 d . . . . .
H1A H 0.452994 0.326779 0.119982 0.027 Uiso 1 1 calc R U . . .
H1B H 0.379608 0.354217 0.169442 0.027 Uiso 1 1 calc R U . . .
H1C H 0.452533 0.358078 0.275253 0.027 Uiso 1 1 calc R U . . .
C11 C 0.5058(7) 0.0796(5) 0.101(3) 0.020(3) Uani 1 1 d . . . . .
H11A H 0.523009 0.072907 0.218661 0.024 Uiso 1 1 calc R U . . .
H11B H 0.449345 0.069289 0.089762 0.024 Uiso 1 1 calc R U . . .
C7 C 0.2397(7) 0.4236(5) 0.583(3) 0.023(4) Uani 1 1 d . . . . .
H7A H 0.295406 0.432765 0.555598 0.028 Uiso 1 1 calc R U . . .
H7B H 0.229314 0.433750 0.701575 0.028 Uiso 1 1 calc R U . . .
C10 C 0.5140(7) 0.1349(5) 0.062(2) 0.019(4) Uani 1 1 d . . . . .
H10A H 0.569756 0.145740 0.080715 0.023 Uiso 1 1 calc R U . . .
H10B H 0.500198 0.141287 -0.057800 0.023 Uiso 1 1 calc R U . . .
C14 C 0.2858(7) 0.1027(5) 0.561(2) 0.0193(18) Uani 1 1 d . . . . .
H14A H 0.307160 0.072138 0.614817 0.023 Uiso 1 1 calc R U . . .
H14B H 0.308950 0.105289 0.446050 0.023 Uiso 1 1 calc R U . . .
C2 C 0.4605(7) 0.3993(5) 0.066(2) 0.018(4) Uani 1 1 d . . . . .
H2A H 0.442960 0.430534 0.122563 0.022 Uiso 1 1 calc R U . . .
H2B H 0.435887 0.398102 -0.047298 0.022 Uiso 1 1 calc R U . . .
C3 C 0.5513(7) 0.3993(6) 0.050(2) 0.021(4) Uani 1 1 d . . . . .
H3A H 0.575409 0.400243 0.163698 0.025 Uiso 1 1 calc R U . . .
H3B H 0.568348 0.367877 -0.005899 0.025 Uiso 1 1 calc R U . . .
C15 C 0.1963(7) 0.0988(5) 0.548(2) 0.0193(18) Uani 1 1 d . . . . .
H15A H 0.174695 0.129823 0.496902 0.023 Uiso 1 1 calc R U . . .
H15B H 0.173164 0.095265 0.662446 0.023 Uiso 1 1 calc R U . . .
C6 C 0.2299(7) 0.3678(6) 0.567(2) 0.021(4) Uani 1 1 d . . . . .
H6A H 0.174816 0.358547 0.599364 0.025 Uiso 1 1 calc R U . . .
H6B H 0.238295 0.357871 0.448188 0.025 Uiso 1 1 calc R U . . .
C4 C 0.5810(9) 0.4428(6) -0.051(3) 0.027(4) Uani 1 1 d . . . . .
H4A H 0.558544 0.440897 -0.166698 0.033 Uiso 1 1 calc R U . . .
H4B H 0.639721 0.440435 -0.060794 0.033 Uiso 1 1 calc R U . . .
C12 C 0.5563(10) 0.0506(6) -0.020(2) 0.030(5) Uani 1 1 d . . . . .
H12A H 0.612839 0.060488 -0.006416 0.036 Uiso 1 1 calc R U . . .
H12B H 0.539939 0.058141 -0.137363 0.036 Uiso 1 1 calc R U . . .
C8 C 0.1837(9) 0.4518(6) 0.467(2) 0.031(5) Uani 1 1 d . . . . .
H8A H 0.128071 0.442209 0.492645 0.038 Uiso 1 1 calc R U . . .
H8B H 0.194952 0.442358 0.348099 0.038 Uiso 1 1 calc R U . . .
C16 C 0.1724(8) 0.0539(5) 0.440(2) 0.0193(18) Uani 1 1 d . . . . .
H16A H 0.197918 0.056721 0.327072 0.023 Uiso 1 1 calc R U . . .
H16B H 0.113916 0.054139 0.422746 0.023 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br2 3.0597(18) . ?
Pb1 Br5 3.045(2) . ?
Pb1 Br6 2.9842(17) 3 ?
Pb1 Br1 2.967(2) . ?
Pb1 Br3 2.9616(16) . ?
Pb1 Br4 3.0229(16) . ?
Pb2 Br2 3.044(2) 1_556 ?
Pb2 Br5 3.0678(19) . ?
Pb2 Br6 2.969(2) . ?
Pb2 Br1 2.9794(18) 3_456 ?
Pb2 Br7 3.0602(17) . ?
Pb2 Br8 2.9303(16) . ?
Cl3 C12 1.831(16) . ?
Cl4 C16 1.808(15) . ?
Cl2 C8 1.768(17) . ?
Cl1 C4 1.819(16) . ?
N9 H9A 0.9100 . ?
N9 H9B 0.9100 . ?
N9 H9C 0.9100 . ?
N9 C10 1.484(17) . ?
N5 H5A 0.9100 . ?
N5 H5B 0.9100 . ?
N5 H5C 0.9100 . ?
N5 C6 1.479(17) . ?
N13 H13A 0.9100 . ?
N13 H13B 0.9100 . ?
N13 H13C 0.9100 . ?
N13 C14 1.506(17) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 H1C 0.9100 . ?
N1 C2 1.493(18) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C10 1.518(18) . ?
C11 C12 1.49(2) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C6 1.51(2) . ?
C7 C8 1.51(2) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C15 1.509(17) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.529(17) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.50(2) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C16 1.53(2) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br5 Pb1 Br2 82.76(6) . . ?
Br6 Pb1 Br2 174.46(6) 3 . ?
Br6 Pb1 Br5 102.34(6) 3 . ?
Br6 Pb1 Br4 93.42(4) 3 . ?
Br1 Pb1 Br2 84.57(6) . . ?
Br1 Pb1 Br5 167.06(5) . . ?
Br1 Pb1 Br6 90.42(5) . 3 ?
Br1 Pb1 Br4 91.94(6) . . ?
Br3 Pb1 Br2 85.40(4) . . ?
Br3 Pb1 Br5 88.05(5) . . ?
Br3 Pb1 Br6 96.84(4) . 3 ?
Br3 Pb1 Br1 88.35(6) . . ?
Br3 Pb1 Br4 169.73(4) . . ?
Br4 Pb1 Br2 84.41(4) . . ?
Br4 Pb1 Br5 89.42(5) . . ?
Br2 Pb2 Br5 82.71(6) 1_556 . ?
Br2 Pb2 Br7 89.41(5) 1_556 . ?
Br6 Pb2 Br2 166.53(5) . 1_556 ?
Br6 Pb2 Br5 84.16(6) . . ?
Br6 Pb2 Br1 90.59(5) . 3_456 ?
Br6 Pb2 Br7 92.34(5) . . ?
Br1 Pb2 Br2 102.46(6) 3_456 1_556 ?
Br1 Pb2 Br5 174.63(6) 3_456 . ?
Br1 Pb2 Br7 96.83(4) 3_456 . ?
Br7 Pb2 Br5 84.57(4) . . ?
Br8 Pb2 Br2 88.09(5) . 1_556 ?
Br8 Pb2 Br5 85.18(4) . . ?
Br8 Pb2 Br6 87.82(6) . . ?
Br8 Pb2 Br1 93.48(5) . 3_456 ?
Br8 Pb2 Br7 169.68(5) . . ?
Pb2 Br2 Pb1 157.12(7) 1_554 . ?
Pb1 Br5 Pb2 157.05(7) . . ?
Pb2 Br6 Pb1 138.27(7) . 3_455 ?
Pb1 Br1 Pb2 138.16(6) . 3_554 ?
H9A N9 H9B 109.5 . . ?
H9A N9 H9C 109.5 . . ?
H9B N9 H9C 109.5 . . ?
C10 N9 H9A 109.5 . . ?
C10 N9 H9B 109.5 . . ?
C10 N9 H9C 109.5 . . ?
H5A N5 H5B 109.5 . . ?
H5A N5 H5C 109.5 . . ?
H5B N5 H5C 109.5 . . ?
C6 N5 H5A 109.5 . . ?
C6 N5 H5B 109.5 . . ?
C6 N5 H5C 109.5 . . ?
H13A N13 H13B 109.5 . . ?
H13A N13 H13C 109.5 . . ?
H13B N13 H13C 109.5 . . ?
C14 N13 H13A 109.5 . . ?
C14 N13 H13B 109.5 . . ?
C14 N13 H13C 109.5 . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C2 N1 H1A 109.5 . . ?
C2 N1 H1B 109.5 . . ?
C2 N1 H1C 109.5 . . ?
H11A C11 H11B 108.3 . . ?
C10 C11 H11A 109.9 . . ?
C10 C11 H11B 109.9 . . ?
C12 C11 H11A 109.9 . . ?
C12 C11 H11B 109.9 . . ?
C12 C11 C10 108.9(15) . . ?
H7A C7 H7B 107.9 . . ?
C6 C7 H7A 109.2 . . ?
C6 C7 H7B 109.2 . . ?
C6 C7 C8 112.0(13) . . ?
C8 C7 H7A 109.2 . . ?
C8 C7 H7B 109.2 . . ?
N9 C10 C11 108.9(13) . . ?
N9 C10 H10A 109.9 . . ?
N9 C10 H10B 109.9 . . ?
C11 C10 H10A 109.9 . . ?
C11 C10 H10B 109.9 . . ?
H10A C10 H10B 108.3 . . ?
N13 C14 H14A 109.5 . . ?
N13 C14 H14B 109.5 . . ?
N13 C14 C15 110.8(11) . . ?
H14A C14 H14B 108.1 . . ?
C15 C14 H14A 109.5 . . ?
C15 C14 H14B 109.5 . . ?
N1 C2 H2A 109.6 . . ?
N1 C2 H2B 109.6 . . ?
N1 C2 C3 110.2(11) . . ?
H2A C2 H2B 108.1 . . ?
C3 C2 H2A 109.6 . . ?
C3 C2 H2B 109.6 . . ?
C2 C3 H3A 109.2 . . ?
C2 C3 H3B 109.2 . . ?
H3A C3 H3B 107.9 . . ?
C4 C3 C2 112.2(12) . . ?
C4 C3 H3A 109.2 . . ?
C4 C3 H3B 109.2 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 C16 110.7(12) . . ?
H15A C15 H15B 108.1 . . ?
C16 C15 H15A 109.5 . . ?
C16 C15 H15B 109.5 . . ?
N5 C6 C7 111.8(13) . . ?
N5 C6 H6A 109.3 . . ?
N5 C6 H6B 109.3 . . ?
C7 C6 H6A 109.3 . . ?
C7 C6 H6B 109.3 . . ?
H6A C6 H6B 107.9 . . ?
Cl1 C4 H4A 108.9 . . ?
Cl1 C4 H4B 108.9 . . ?
C3 C4 Cl1 113.4(13) . . ?
C3 C4 H4A 108.9 . . ?
C3 C4 H4B 108.9 . . ?
H4A C4 H4B 107.7 . . ?
Cl3 C12 H12A 109.7 . . ?
Cl3 C12 H12B 109.7 . . ?
C11 C12 Cl3 109.7(12) . . ?
C11 C12 H12A 109.7 . . ?
C11 C12 H12B 109.7 . . ?
H12A C12 H12B 108.2 . . ?
Cl2 C8 H8A 109.4 . . ?
Cl2 C8 H8B 109.4 . . ?
C7 C8 Cl2 111.3(11) . . ?
C7 C8 H8A 109.4 . . ?
C7 C8 H8B 109.4 . . ?
H8A C8 H8B 108.0 . . ?
Cl4 C16 H16A 109.3 . . ?
Cl4 C16 H16B 109.3 . . ?
C15 C16 Cl4 111.7(11) . . ?
C15 C16 H16A 109.3 . . ?
C15 C16 H16B 109.3 . . ?
H16A C16 H16B 107.9 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N9 H9A Br8 0.91 2.48 3.385(11) 177.4 1_554 yes
N9 H9B Br5 0.91 2.84 3.413(12) 122.3 1_554 yes
N9 H9B Br1 0.91 2.69 3.429(12) 138.9 . yes
N9 H9C Br4 0.91 2.44 3.341(12) 169.5 . yes
N5 H5A Br3 0.91 2.48 3.390(10) 174.5 . yes
N5 H5B Br2 0.91 2.77 3.407(12) 127.6 . yes
N5 H5B Br6 0.91 2.76 3.446(12) 133.2 . yes
N5 H5C Br7 0.91 2.44 3.348(12) 174.6 . yes
N13 H13A Br2 0.91 2.82 3.489(13) 131.6 . yes
N13 H13A Br6 0.91 2.82 3.469(12) 129.2 . yes
N13 H13B Br4 0.91 2.45 3.329(11) 162.9 . yes
N13 H13C Br8 0.91 2.50 3.407(13) 171.1 . yes
N1 H1A Br5 0.91 2.76 3.474(13) 136.6 1_554 yes
N1 H1A Br1 0.91 2.88 3.496(12) 126.0 . yes
N1 H1B Br7 0.91 2.45 3.325(11) 161.8 1_554 yes
N1 H1C Br3 0.91 2.49 3.388(13) 170.1 . yes

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
N13 C14 C15 C16 178.4(13) . . . . ?
N1 C2 C3 C4 -180.0(13) . . . . ?
C10 C11 C12 Cl3 -178.6(11) . . . . ?
C14 C15 C16 Cl4 64.9(15) . . . . ?
C2 C3 C4 Cl1 60.2(17) . . . . ?
C6 C7 C8 Cl2 178.7(12) . . . . ?
C12 C11 C10 N9 176.3(13) . . . . ?
C8 C7 C6 N5 177.8(14) . . . . ?

_olex2_date_sample_data_collection 2023-11-20
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.488
_oxdiff_exptl_absorpt_empirical_full_min 0.589
