# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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_immhypbbr4_295k
_database_code_depnum_ccdc_archive 'CCDC 2182360'
loop_
_audit_author_name
_audit_author_address
'Dawid Drozdowski'
;Institute of Low Temperature and Structure Research Polish Academy of Sciences
Poland
;
_audit_update_record             
;
2023-01-05 deposited with the CCDC.	2023-03-13 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT342_immhypbbr4_295k     
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............       0.03 Ang.
RESPONSE: Disorder of the organic moieties.
;
# Added during the CSD deposition process: Thursday 05 January 2023 11:35 AM
# end Validation Reply Form

_audit_creation_date             2023-01-05
_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, C3 H5 N2, C H5 N1.333, 0.667(N)'
_chemical_formula_sum            'C4 H10 Br4 N4 Pb'
_chemical_formula_weight         640.99
_chemical_melting_point          ?
_chemical_oxdiff_formula         PbBr4N4C4H12
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   5.9753(7)
_cell_length_b                   28.414(4)
_cell_length_c                   8.2762(12)
_cell_angle_alpha                90
_cell_angle_beta                 90.489(12)
_cell_angle_gamma                90
_cell_volume                     1405.1(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1504
_cell_measurement_temperature    295
_cell_measurement_theta_max      29.0800
_cell_measurement_theta_min      2.5540
_shelx_estimated_absorpt_T_max   0.292
_shelx_estimated_absorpt_T_min   0.089
_exptl_absorpt_coefficient_mu    23.352
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.27954
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
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    3.030
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_unetI/netI     0.0643
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            6467
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_min         2.563
_diffrn_ambient_temperature      295
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6249
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -12.00  69.00   1.00   18.00    --   13.31  77.00 -60.00   81
  2  ω    -42.00  15.00   1.00   18.00    --  -14.40  57.00  90.00   57
;
_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      0.0970943000
_diffrn_orient_matrix_UB_12      -0.0026540000
_diffrn_orient_matrix_UB_13      0.0487101000
_diffrn_orient_matrix_UB_21      0.0676107000
_diffrn_orient_matrix_UB_22      0.0037371000
_diffrn_orient_matrix_UB_23      -0.0682411000
_diffrn_orient_matrix_UB_31      0.0002361000
_diffrn_orient_matrix_UB_32      0.0244375000
_diffrn_orient_matrix_UB_33      0.0158303000
_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                2188
_reflns_number_total             2846
_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 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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    ?
_refine_diff_density_max         1.588
_refine_diff_density_min         -2.388
_refine_diff_density_rms         0.251
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     114
_refine_ls_number_reflns         2846
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0832
_refine_ls_R_factor_gt           0.0573
_refine_ls_restrained_S_all      1.091
_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)+(0.0443P)²+8.7789P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1115
_refine_ls_wR_factor_ref         0.1237
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N6) = Uanis(N7A) = Uanis(N7C) = Uanis(N7B) = Uanis(C8)
3. Others
 Fixed Sof: N7A(0.33333) N7C(0.33333) N7B(0.33333)
4.a Rotating group:
 N6(H6A,H6B)
4.b Aromatic/amide H refined with riding coordinates:
 N4(H4), C3(H3), N1(H1), C2(H2), C5(H5)
4.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C)
;
_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 0.49345(8) 0.17200(2) 0.70837(6) 0.03360(18) Uani 1 1 d . . . . .
Br1 Br 0.4895(3) 0.10968(6) 0.99826(19) 0.0629(5) Uani 1 1 d . . . . .
Br2 Br 0.4870(3) 0.09213(6) 0.4962(2) 0.0602(4) Uani 1 1 d . . . . .
Br3 Br 0.4932(3) 0.23372(6) 0.4123(2) 0.0704(5) Uani 1 1 d . . . . .
Br4 Br -0.0061(2) 0.16518(6) 0.7053(3) 0.0742(6) Uani 1 1 d . . . . .
N4 N -0.072(3) -0.0373(6) 0.273(2) 0.096(5) Uani 1 1 d . . . . .
H4 H -0.136886 -0.063572 0.295114 0.115 Uiso 1 1 calc R U . . .
C3 C 0.124(3) -0.0324(7) 0.203(2) 0.075(5) Uani 1 1 d . . . . .
H3 H 0.217820 -0.056346 0.167488 0.090 Uiso 1 1 calc R U . . .
N1 N -0.008(4) 0.0350(6) 0.256(2) 0.099(6) Uani 1 1 d . . . . .
H1 H -0.021371 0.065024 0.264917 0.118 Uiso 1 1 calc R U . . .
C2 C 0.161(4) 0.0132(10) 0.192(3) 0.095(7) Uani 1 1 d . . . . .
H2 H 0.285689 0.027361 0.145933 0.114 Uiso 1 1 calc R U . . .
C5 C -0.150(4) 0.0046(10) 0.304(3) 0.101(7) Uani 1 1 d . . . . .
H5 H -0.286203 0.011247 0.353293 0.121 Uiso 1 1 calc R U . . .
N6 N -0.023(4) 0.1349(6) 0.276(2) 0.115(5) Uani 1 1 d . . . . .
H6A H 0.098157 0.139088 0.337561 0.138 Uiso 1 1 d R U . . .
H6B H -0.144153 0.143217 0.331180 0.138 Uiso 1 1 d R U . . .
C8 C -0.002(4) 0.2089(8) 0.143(3) 0.115(5) Uani 1 1 d . . . . .
H8A H 0.106874 0.223441 0.074388 0.172 Uiso 1 1 calc R U . . .
H8B H 0.028241 0.217259 0.253365 0.172 Uiso 1 1 calc R U . . .
H8C H -0.148890 0.219432 0.112737 0.172 Uiso 1 1 calc R U . . .
N7A N 0.093(13) 0.169(2) 0.218(8) 0.115(5) Uani 0.3333 1 d . . P . .
N7C N -0.111(12) 0.169(2) 0.205(8) 0.115(5) Uani 0.3333 1 d . . P . .
N7B N 0.009(13) 0.165(2) 0.128(8) 0.115(5) Uani 0.3333 1 d . . 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 Br1 2.9821(16) . ?
Pb1 Br2 2.8697(16) . ?
Pb1 Br3 3.1661(17) 4_566 ?
Pb1 Br3 3.0134(16) . ?
Pb1 Br4 2.9909(15) . ?
Pb1 Br4 2.9972(15) 1_655 ?
N4 H4 0.8600 . ?
N4 C3 1.32(2) . ?
N4 C5 1.31(3) . ?
C3 H3 0.9300 . ?
C3 C2 1.32(3) . ?
N1 H1 0.8600 . ?
N1 C2 1.30(3) . ?
N1 C5 1.28(3) . ?
C2 H2 0.9300 . ?
C5 H5 0.9300 . ?
N6 H6A 0.8902 . ?
N6 H6B 0.8903 . ?
N6 N7B 1.51(6) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C8 N7B 1.26(6) . ?
N7A H6A 1.3084 . ?
N7C H6B 1.2923 . ?

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 179.03(5) . . ?
Br1 Pb1 Br3 94.22(5) . 4_566 ?
Br1 Pb1 Br4 87.33(5) . . ?
Br1 Pb1 Br4 89.03(6) . 1_655 ?
Br2 Pb1 Br1 91.30(5) . . ?
Br2 Pb1 Br3 87.86(5) . . ?
Br2 Pb1 Br3 174.42(5) . 4_566 ?
Br2 Pb1 Br4 86.30(5) . . ?
Br2 Pb1 Br4 87.24(5) . 1_655 ?
Br3 Pb1 Br3 86.621(19) . 4_566 ?
Br4 Pb1 Br3 93.11(5) . 4_566 ?
Br4 Pb1 Br3 91.40(6) 1_655 . ?
Br4 Pb1 Br3 93.69(5) 1_655 4_566 ?
Br4 Pb1 Br3 92.13(6) . . ?
Br4 Pb1 Br4 172.51(7) . 1_655 ?
Pb1 Br3 Pb1 157.79(7) . 4_565 ?
Pb1 Br4 Pb1 172.51(7) . 1_455 ?
C3 N4 H4 126.0 . . ?
C5 N4 H4 126.0 . . ?
C5 N4 C3 108.0(18) . . ?
N4 C3 H3 126.7 . . ?
C2 C3 N4 106.5(18) . . ?
C2 C3 H3 126.7 . . ?
C2 N1 H1 125.5 . . ?
C5 N1 H1 125.5 . . ?
C5 N1 C2 109(2) . . ?
C3 C2 H2 126.0 . . ?
N1 C2 C3 108.0(19) . . ?
N1 C2 H2 126.0 . . ?
N4 C5 H5 125.8 . . ?
N1 C5 N4 108(2) . . ?
N1 C5 H5 125.8 . . ?
H6A N6 H6B 109.4 . . ?
N7B N6 H6A 106.2 . . ?
N7B N6 H6B 112.1 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N7B C8 H8A 109.5 . . ?
N7B C8 H8B 109.5 . . ?
N7B C8 H8C 109.5 . . ?
C8 N7B N6 118(5) . . ?

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
N4 H4 Br2 0.86 2.84 3.506(18) 135.2 3_556 yes
C3 H3 Br1 0.93 2.70 3.604(18) 164.8 3_656 yes
N1 H1 N6 0.86 1.99 2.84(3) 174.4 . yes
C2 H2 Br1 0.93 2.91 3.74(2) 149.1 1_554 yes
C5 H5 Br2 0.93 2.92 3.67(2) 138.2 1_455 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
N4 C3 C2 N1 1(2) . . . . ?
C3 N4 C5 N1 0(3) . . . . ?
C2 N1 C5 N4 1(3) . . . . ?
C5 N4 C3 C2 0(2) . . . . ?
C5 N1 C2 C3 -1(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 2.346
_oxdiff_exptl_absorpt_empirical_full_min 0.597
####################################################################### 
# 
# 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_immhypbcl4_390k
_database_code_depnum_ccdc_archive 'CCDC 2182518'
loop_
_audit_author_name
_audit_author_address
'Dawid Drozdowski'
;Institute of Low Temperature and Structure Research Polish Academy of Sciences
Poland
;
_audit_update_record             
;
2022-12-09 deposited with the CCDC.	2023-03-13 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_immhypbcl4_390k     
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.899 Why?
RESPONSE: Crystal decomposes in the measurement temperature.
;
_vrf_PLAT242_immhypbcl4_390k     
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        Pb1 Check
RESPONSE: Chlorines connected to Pb1 exhibit high thermal dynamics.
;
# Added during the CSD deposition process: Friday 09 December 2022 09:43 AM
# end Validation Reply Form

_audit_creation_date             2022-12-09
_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         'Cl4 Pb, 0.5(C2 N4), C3 N2'
_chemical_formula_sum            'C4 Cl4 N4 Pb'
_chemical_formula_weight         453.07
_chemical_melting_point          ?
_chemical_oxdiff_formula         C4N4PbCl4
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'
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           13
_space_group_name_H-M_alt        'P 1 2/c 1'
_space_group_name_Hall           '-P 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'

_cell_length_a                   5.7615(4)
_cell_length_b                   13.7246(13)
_cell_length_c                   8.1876(9)
_cell_angle_alpha                90
_cell_angle_beta                 90.468(9)
_cell_angle_gamma                90
_cell_volume                     647.41(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    831
_cell_measurement_temperature    390.1(2)
_cell_measurement_theta_max      24.1720
_cell_measurement_theta_min      3.8600
_shelx_estimated_absorpt_T_max   0.770
_shelx_estimated_absorpt_T_min   0.231
_exptl_absorpt_coefficient_mu    13.820
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.14518
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    2.324
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             404
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_av_unetI/netI     0.0685
_diffrn_reflns_Laue_measured_fraction_full 0.899
_diffrn_reflns_Laue_measured_fraction_max 0.893
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            2397
_diffrn_reflns_point_group_measured_fraction_full 0.899
_diffrn_reflns_point_group_measured_fraction_max 0.893
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.667
_diffrn_reflns_theta_min         2.897
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      390.1(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6249
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.899
_diffrn_measured_fraction_theta_max 0.893
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -23.00  97.00   1.00   12.00    --   13.31  77.00  30.00  120
  2  ω    -23.00  27.00   1.00   12.00    --   13.31  77.00-120.00   50
;
_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      -0.0018523000
_diffrn_orient_matrix_UB_12      -0.0350059000
_diffrn_orient_matrix_UB_13      0.0636204000
_diffrn_orient_matrix_UB_21      0.0200180000
_diffrn_orient_matrix_UB_22      0.0374119000
_diffrn_orient_matrix_UB_23      0.0582223000
_diffrn_orient_matrix_UB_31      -0.1215449000
_diffrn_orient_matrix_UB_32      0.0066701000
_diffrn_orient_matrix_UB_33      0.0078583000
_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                874
_reflns_number_total             1093
_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 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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         0.829
_refine_diff_density_min         -1.159
_refine_diff_density_rms         0.185
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     59
_refine_ls_number_reflns         1093
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0676
_refine_ls_R_factor_gt           0.0467
_refine_ls_restrained_S_all      1.033
_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)+(0.0527P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0971
_refine_ls_wR_factor_ref         0.1119
_refine_special_details          ?
_olex2_refinement_description    
;
1. Shared sites
{C3, N3}
{C4, N4}
{C5, N5}
{C6, N6}
{C7, N7}
2. Restrained distances
 N2-N1 = N1-C1
 1.4 with sigma of 0.001
3. Restrained planarity
 C3, C4, C5, C6, C7, N3, N4, N5, N6, N7
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uiso(C1) = Uiso(N1) = Uiso(N2)
Uiso(C3) = Uiso(N3)
Uiso(C4) = Uiso(N4)
Uiso(C5) = Uiso(N5)
Uiso(C6) = Uiso(N6)
Uiso(C7) = Uiso(N7)
5. Others
 Fixed Sof: Cl2(0.5) N1(0.5) C1(0.5) N2(0.5) C3(0.3) C4(0.3) C5(0.3) C6(0.3)
 C7(0.3) N3(0.2) N4(0.2) N5(0.2) N6(0.2) N7(0.2)
;
_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 0.000000 0.34387(4) 0.250000 0.0571(3) Uani 1 2 d S T P . .
Cl1 Cl 0.500000 0.3332(6) 0.250000 0.128(3) Uani 1 2 d S T P . .
Cl3 Cl 0.0039(10) 0.2037(4) 0.4909(6) 0.1245(18) Uani 1 1 d . . . . .
Cl2 Cl -0.039(9) 0.488(4) 0.522(5) 0.169(8) Uani 0.5 1 d . . P . .
N1 N 0.467(6) 0.4009(17) 0.697(8) 0.25(3) Uiso 0.5 1 d D . P . .
C1 C 0.671(6) 0.347(3) 0.718(12) 0.25(3) Uiso 0.5 1 d D . P . .
N2 N 0.503(13) 0.3008(17) 0.678(7) 0.25(3) Uiso 0.5 1 d D . P . .
C3 C 0.439(8) 0.078(3) 0.274(5) 0.120(19) Uiso 0.3 1 d . . P . .
C4 C 0.444(6) -0.079(2) 0.269(5) 0.102(12) Uiso 0.3 1 d . . P . .
C5 C 0.326(9) 0.006(5) 0.317(5) 0.15(2) Uiso 0.3 1 d . . P . .
C6 C 0.355(7) -0.046(4) 0.306(4) 0.121(14) Uiso 0.3 1 d . . P . .
C7 C 0.367(8) 0.054(4) 0.298(4) 0.110(15) Uiso 0.3 1 d . . P . .
N3 N 0.439(8) 0.078(3) 0.274(5) 0.120(19) Uiso 0.2 1 d . . P . .
N4 N 0.444(6) -0.079(2) 0.269(5) 0.102(12) Uiso 0.2 1 d . . P . .
N5 N 0.326(9) 0.006(5) 0.317(5) 0.15(2) Uiso 0.2 1 d . . P . .
N6 N 0.355(7) -0.046(4) 0.306(4) 0.121(14) Uiso 0.2 1 d . . P . .
N7 N 0.367(8) 0.054(4) 0.298(4) 0.110(15) Uiso 0.2 1 d . . 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 Cl1 2.8844(4) . ?
Pb1 Cl1 2.8844(4) 1_455 ?
Pb1 Cl3 2.755(4) . ?
Pb1 Cl3 2.755(4) 2 ?
Pb1 Cl2 2.98(4) 4_565 ?
Pb1 Cl2 2.99(4) 2 ?
Pb1 Cl2 2.98(4) 3_566 ?
Pb1 Cl2 2.99(4) . ?
Cl2 Cl2 0.67(4) 3_566 ?
N1 N1 0.94(11) 2_656 ?
N1 C1 1.29(7) 2_656 ?
N1 C1 1.4000(11) . ?
N1 N2 1.4000(10) . ?
N1 N2 1.72(6) 2_656 ?
C1 C1 2.04(9) 2_656 ?
C1 N2 1.46(7) 2_656 ?
C1 N2 1.20(7) . ?
N2 N2 1.19(11) 2_656 ?
C3 C3 0.80(9) 2_655 ?
C3 C5 1.24(7) . ?
C3 C5 1.84(7) 2_655 ?
C3 C6 1.79(6) . ?
C3 C7 0.57(6) . ?
C3 C7 1.31(7) 2_655 ?
C4 C4 0.72(7) 2_655 ?
C4 C5 1.91(7) 2_655 ?
C4 C5 1.41(7) . ?
C4 C6 0.76(5) . ?
C4 C6 1.40(6) 2_655 ?
C4 C7 1.89(6) . ?
C5 C6 0.73(8) . ?
C5 C7 0.72(8) . ?
C6 C6 1.92(9) 2_655 ?
C6 C7 1.37(9) . ?
C7 C7 1.73(10) 2_655 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1 Pb1 Cl1 174.2(3) . 1_455 ?
Cl1 Pb1 Cl2 87.3(9) 1_455 . ?
Cl1 Pb1 Cl2 96.3(9) . 4_565 ?
Cl1 Pb1 Cl2 96.6(10) . . ?
Cl1 Pb1 Cl2 96.6(10) 1_455 2 ?
Cl1 Pb1 Cl2 87.3(9) . 2 ?
Cl1 Pb1 Cl2 88.2(10) 1_455 4_565 ?
Cl1 Pb1 Cl2 88.2(10) . 3_566 ?
Cl1 Pb1 Cl2 96.3(9) 1_455 3_566 ?
Cl3 Pb1 Cl1 88.10(16) 2 . ?
Cl3 Pb1 Cl1 87.85(16) 2 1_455 ?
Cl3 Pb1 Cl1 88.10(16) . 1_455 ?
Cl3 Pb1 Cl1 87.85(16) . . ?
Cl3 Pb1 Cl3 91.4(3) . 2 ?
Cl3 Pb1 Cl2 95.4(9) . 3_566 ?
Cl3 Pb1 Cl2 174.5(5) . 2 ?
Cl3 Pb1 Cl2 174.5(5) 2 . ?
Cl3 Pb1 Cl2 172.1(5) 2 3_566 ?
Cl3 Pb1 Cl2 85.8(10) 2 2 ?
Cl3 Pb1 Cl2 172.1(5) . 4_565 ?
Cl3 Pb1 Cl2 95.4(9) 2 4_565 ?
Cl3 Pb1 Cl2 85.8(10) . . ?
Cl2 Pb1 Cl2 13.0(8) 4_565 2 ?
Cl2 Pb1 Cl2 87.05(18) 4_565 . ?
Cl2 Pb1 Cl2 97.4(18) . 2 ?
Cl2 Pb1 Cl2 87.05(19) 3_566 2 ?
Cl2 Pb1 Cl2 78(2) 3_566 4_565 ?
Cl2 Pb1 Cl2 13.0(8) 3_566 . ?
Pb1 Cl1 Pb1 174.2(3) . 1_655 ?
Pb1 Cl2 Pb1 167.0(8) 3_566 . ?
Cl2 Cl2 Pb1 83(7) 3_566 . ?
Cl2 Cl2 Pb1 84(7) 3_566 3_566 ?
N1 N1 C1 76(6) 2_656 2_656 ?
N1 N1 C1 63(4) 2_656 . ?
N1 N1 N2 93(3) 2_656 . ?
N1 N1 N2 54(3) 2_656 2_656 ?
C1 N1 C1 98(5) 2_656 . ?
C1 N1 N2 51(3) . . ?
C1 N1 N2 66(4) 2_656 . ?
C1 N1 N2 44(3) 2_656 2_656 ?
C1 N1 N2 55(4) . 2_656 ?
N2 N1 N2 43(4) . 2_656 ?
N1 C1 N1 41(5) 2_656 . ?
N1 C1 C1 43(3) 2_656 2_656 ?
N1 C1 C1 39(3) . 2_656 ?
N1 C1 N2 61(3) 2_656 2_656 ?
N1 C1 N2 74(4) . 2_656 ?
N2 C1 N1 64.7(16) . . ?
N2 C1 N1 88(4) . 2_656 ?
N2 C1 C1 45(2) . 2_656 ?
N2 C1 C1 35(3) 2_656 2_656 ?
N2 C1 N2 52(5) . 2_656 ?
N1 N2 N1 33(4) . 2_656 ?
N1 N2 C1 54(3) . 2_656 ?
C1 N2 N1 51.3(16) 2_656 2_656 ?
C1 N2 N1 49(3) . 2_656 ?
C1 N2 N1 64.7(16) . . ?
C1 N2 C1 100(4) . 2_656 ?
N2 N2 N1 83(3) 2_656 . ?
N2 N2 N1 54(3) 2_656 2_656 ?
N2 N2 C1 52(5) 2_656 2_656 ?
N2 N2 C1 76(7) 2_656 . ?
C3 C3 C5 33(2) 2_655 2_655 ?
C3 C3 C5 127(3) 2_655 . ?
C3 C3 C6 108(2) 2_655 . ?
C3 C3 C7 15(3) 2_655 2_655 ?
C5 C3 C5 95(5) . 2_655 ?
C5 C3 C6 19(3) . . ?
C5 C3 C7 112(5) . 2_655 ?
C6 C3 C5 76(3) . 2_655 ?
C7 C3 C3 144(9) . 2_655 ?
C7 C3 C5 18(8) . . ?
C7 C3 C5 18(4) 2_655 2_655 ?
C7 C3 C5 112(9) . 2_655 ?
C7 C3 C6 94(4) 2_655 . ?
C7 C3 C6 36(8) . . ?
C7 C3 C7 130(10) . 2_655 ?
C4 C4 C5 124(3) 2_655 . ?
C4 C4 C5 38(2) 2_655 2_655 ?
C4 C4 C6 19(3) 2_655 2_655 ?
C4 C4 C6 142(5) 2_655 . ?
C4 C4 C7 105.5(19) 2_655 . ?
C5 C4 C5 86(4) . 2_655 ?
C5 C4 C7 19(3) . . ?
C6 C4 C5 19(3) 2_655 2_655 ?
C6 C4 C5 105(4) 2_655 . ?
C6 C4 C5 19(6) . . ?
C6 C4 C5 105(5) . 2_655 ?
C6 C4 C6 124(8) . 2_655 ?
C6 C4 C7 86(3) 2_655 . ?
C6 C4 C7 37(5) . . ?
C7 C4 C5 68(3) . 2_655 ?
C3 C5 C3 20(3) . 2_655 ?
C3 C5 C4 109(5) . . ?
C3 C5 C4 91(4) . 2_655 ?
C3 C5 C4 70(3) 2_655 2_655 ?
C4 C5 C3 88(3) . 2_655 ?
C4 C5 C4 18(2) . 2_655 ?
C6 C5 C3 108(8) . 2_655 ?
C6 C5 C3 128(9) . . ?
C6 C5 C4 19(5) . . ?
C6 C5 C4 37(6) . 2_655 ?
C7 C5 C3 34(6) . 2_655 ?
C7 C5 C3 14(6) . . ?
C7 C5 C4 122(9) . . ?
C7 C5 C4 104(8) . 2_655 ?
C7 C5 C6 142(10) . . ?
C3 C6 C6 72(2) . 2_655 ?
C4 C6 C3 109(6) . . ?
C4 C6 C3 91(3) 2_655 . ?
C4 C6 C4 18(3) . 2_655 ?
C4 C6 C6 19(3) 2_655 2_655 ?
C4 C6 C6 37(5) . 2_655 ?
C4 C6 C7 123(6) . . ?
C5 C6 C3 33(6) . . ?
C5 C6 C4 124(9) . 2_655 ?
C5 C6 C4 142(10) . . ?
C5 C6 C6 105(7) . 2_655 ?
C5 C6 C7 19(7) . . ?
C7 C6 C3 14(3) . . ?
C7 C6 C4 105(4) . 2_655 ?
C7 C6 C6 86(3) . 2_655 ?
C3 C7 C3 21(6) . 2_655 ?
C3 C7 C4 110(9) . . ?
C3 C7 C4 89(4) 2_655 . ?
C3 C7 C5 149(10) . . ?
C3 C7 C6 129(10) . . ?
C3 C7 C6 109(5) 2_655 . ?
C3 C7 C7 36(9) . 2_655 ?
C3 C7 C7 15(3) 2_655 2_655 ?
C5 C7 C3 128(9) . 2_655 ?
C5 C7 C4 39(7) . . ?
C5 C7 C6 19(7) . . ?
C5 C7 C7 113(8) . 2_655 ?
C6 C7 C4 20(2) . . ?
C6 C7 C7 94(3) . 2_655 ?
C7 C7 C4 74.5(19) 2_655 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 N1 C1 C1 70(6) 2_656 . . 2_656 ?
N1 N1 C1 N2 118(6) 2_656 . . . ?
N1 N1 C1 N2 63(4) 2_656 . . 2_656 ?
N1 N1 N2 C1 -52(6) 2_656 . . . ?
N1 N1 N2 C1 73(6) 2_656 . . 2_656 ?
N1 N1 N2 N2 25(8) 2_656 . . 2_656 ?
N1 C1 N2 N1 35(5) 2_656 . . . ?
N1 C1 N2 N1 -35(5) . . . 2_656 ?
N1 C1 N2 C1 -7(4) 2_656 . . 2_656 ?
N1 C1 N2 C1 -42(4) . . . 2_656 ?
N1 C1 N2 N2 -89(5) . . . 2_656 ?
N1 C1 N2 N2 -54(4) 2_656 . . 2_656 ?
C1 N1 C1 N1 -70(6) 2_656 . . 2_656 ?
C1 N1 C1 N2 -6(4) 2_656 . . 2_656 ?
C1 N1 C1 N2 49(4) 2_656 . . . ?
C1 N1 N2 N1 -73(6) 2_656 . . 2_656 ?
C1 N1 N2 N1 52(6) . . . 2_656 ?
C1 N1 N2 C1 -125(5) 2_656 . . . ?
C1 N1 N2 C1 125(5) . . . 2_656 ?
C1 N1 N2 N2 -48(6) 2_656 . . 2_656 ?
C1 N1 N2 N2 77(8) . . . 2_656 ?
C1 C1 N2 N1 7(4) 2_656 . . 2_656 ?
C1 C1 N2 N1 42(4) 2_656 . . . ?
C1 C1 N2 N2 -47(4) 2_656 . . 2_656 ?
N2 N1 C1 N1 -63(4) 2_656 . . 2_656 ?
N2 N1 C1 N1 -118(6) . . . 2_656 ?
N2 N1 C1 C1 -49(4) . . . 2_656 ?
N2 N1 C1 C1 6(4) 2_656 . . 2_656 ?
N2 N1 C1 N2 55(5) 2_656 . . . ?
N2 N1 C1 N2 -55(5) . . . 2_656 ?
N2 N1 N2 N1 -25(8) 2_656 . . 2_656 ?
N2 N1 N2 C1 -77(8) 2_656 . . . ?
N2 N1 N2 C1 48(6) 2_656 . . 2_656 ?
N2 C1 N2 N1 89(5) 2_656 . . . ?
N2 C1 N2 N1 54(4) 2_656 . . 2_656 ?
N2 C1 N2 C1 47(4) 2_656 . . 2_656 ?
C3 C3 C5 C4 1(10) 2_655 . . 2_655 ?
C3 C3 C5 C4 -1(12) 2_655 . . . ?
C3 C3 C5 C6 0(13) 2_655 . . . ?
C3 C3 C5 C7 -171(21) 2_655 . . . ?
C3 C3 C6 C4 -1(10) 2_655 . . . ?
C3 C3 C6 C4 1(7) 2_655 . . 2_655 ?
C3 C3 C6 C5 -180(11) 2_655 . . . ?
C3 C3 C6 C6 0(7) 2_655 . . 2_655 ?
C3 C3 C6 C7 -175(14) 2_655 . . . ?
C3 C3 C7 C4 5(20) 2_655 . . . ?
C3 C3 C7 C5 12(28) 2_655 . . . ?
C3 C3 C7 C6 8(23) 2_655 . . . ?
C3 C3 C7 C7 3(11) 2_655 . . 2_655 ?
C3 C5 C6 C3 0(5) 2_655 . . . ?
C3 C5 C6 C4 1(8) . . . 2_655 ?
C3 C5 C6 C4 -3(10) 2_655 . . . ?
C3 C5 C6 C4 1(5) 2_655 . . 2_655 ?
C3 C5 C6 C4 -3(11) . . . . ?
C3 C5 C6 C6 0(4) 2_655 . . 2_655 ?
C3 C5 C6 C6 0(6) . . . 2_655 ?
C3 C5 C6 C7 -3(7) 2_655 . . . ?
C3 C5 C6 C7 -3(6) . . . . ?
C3 C5 C7 C3 5(13) . . . 2_655 ?
C3 C5 C7 C3 -5(13) 2_655 . . . ?
C3 C5 C7 C4 10(16) . . . . ?
C3 C5 C7 C4 5(8) 2_655 . . . ?
C3 C5 C7 C6 5(12) 2_655 . . . ?
C3 C5 C7 C6 11(19) . . . . ?
C3 C5 C7 C7 0(3) 2_655 . . 2_655 ?
C3 C5 C7 C7 6(12) . . . 2_655 ?
C3 C6 C7 C3 3(9) . . . 2_655 ?
C3 C6 C7 C4 7(9) . . . . ?
C3 C6 C7 C5 -173(13) . . . . ?
C3 C6 C7 C7 3(7) . . . 2_655 ?
C4 C4 C5 C3 5(11) 2_655 . . . ?
C4 C4 C5 C3 4(9) 2_655 . . 2_655 ?
C4 C4 C5 C6 -173(16) 2_655 . . . ?
C4 C4 C5 C7 7(12) 2_655 . . . ?
C4 C4 C6 C3 8(18) 2_655 . . . ?
C4 C4 C6 C5 9(21) 2_655 . . . ?
C4 C4 C6 C6 5(11) 2_655 . . 2_655 ?
C4 C4 C6 C7 10(18) 2_655 . . . ?
C4 C4 C7 C3 2(7) 2_655 . . 2_655 ?
C4 C4 C7 C3 0(11) 2_655 . . . ?
C4 C4 C7 C5 -174(11) 2_655 . . . ?
C4 C4 C7 C6 -174(12) 2_655 . . . ?
C4 C4 C7 C7 2(7) 2_655 . . 2_655 ?
C4 C5 C6 C3 -1(8) 2_655 . . . ?
C4 C5 C6 C3 3(11) . . . . ?
C4 C5 C6 C4 4(8) . . . 2_655 ?
C4 C5 C6 C4 -4(8) 2_655 . . . ?
C4 C5 C6 C6 -1(2) 2_655 . . 2_655 ?
C4 C5 C6 C6 3(7) . . . 2_655 ?
C4 C5 C6 C7 -4(11) 2_655 . . . ?
C4 C5 C6 C7 0(14) . . . . ?
C4 C5 C7 C3 -3(6) 2_655 . . 2_655 ?
C4 C5 C7 C3 -8(15) 2_655 . . . ?
C4 C5 C7 C3 -10(16) . . . . ?
C4 C5 C7 C3 -5(8) . . . 2_655 ?
C4 C5 C7 C4 2(4) 2_655 . . . ?
C4 C5 C7 C6 0(6) . . . . ?
C4 C5 C7 C6 3(7) 2_655 . . . ?
C4 C5 C7 C7 -2(4) 2_655 . . 2_655 ?
C4 C5 C7 C7 -5(7) . . . 2_655 ?
C4 C6 C7 C3 -7(9) . . . . ?
C4 C6 C7 C3 -4(7) . . . 2_655 ?
C4 C6 C7 C3 -1(3) 2_655 . . 2_655 ?
C4 C6 C7 C3 -4(9) 2_655 . . . ?
C4 C6 C7 C4 3(6) 2_655 . . . ?
C4 C6 C7 C5 -180(11) . . . . ?
C4 C6 C7 C5 -177(10) 2_655 . . . ?
C4 C6 C7 C7 -1(3) 2_655 . . 2_655 ?
C4 C6 C7 C7 -4(6) . . . 2_655 ?
C5 C3 C5 C3 0(8) 2_655 . . 2_655 ?
C5 C3 C5 C4 -1(4) 2_655 . . . ?
C5 C3 C5 C4 0.7(18) 2_655 . . 2_655 ?
C5 C3 C5 C6 0(5) 2_655 . . . ?
C5 C3 C5 C7 -171(15) 2_655 . . . ?
C5 C3 C6 C4 178(7) . . . . ?
C5 C3 C6 C4 -179(7) . . . 2_655 ?
C5 C3 C6 C4 -2(5) 2_655 . . . ?
C5 C3 C6 C4 1(2) 2_655 . . 2_655 ?
C5 C3 C6 C5 -180(6) 2_655 . . . ?
C5 C3 C6 C6 0.0(16) 2_655 . . 2_655 ?
C5 C3 C6 C6 180(7) . . . 2_655 ?
C5 C3 C6 C7 4(7) . . . . ?
C5 C3 C6 C7 -176(9) 2_655 . . . ?
C5 C3 C7 C3 -3(14) 2_655 . . 2_655 ?
C5 C3 C7 C3 -12(28) . . . 2_655 ?
C5 C3 C7 C4 2(6) 2_655 . . . ?
C5 C3 C7 C4 -7(11) . . . . ?
C5 C3 C7 C5 9(16) 2_655 . . . ?
C5 C3 C7 C6 5(9) 2_655 . . . ?
C5 C3 C7 C6 -5(8) . . . . ?
C5 C3 C7 C7 -9(18) . . . 2_655 ?
C5 C3 C7 C7 0(3) 2_655 . . 2_655 ?
C5 C4 C5 C3 0.6(15) 2_655 . . 2_655 ?
C5 C4 C5 C3 1(3) 2_655 . . . ?
C5 C4 C5 C4 -4(9) 2_655 . . 2_655 ?
C5 C4 C5 C6 -177(10) 2_655 . . . ?
C5 C4 C5 C7 3(5) 2_655 . . . ?
C5 C4 C6 C3 -2(7) . . . . ?
C5 C4 C6 C3 2(5) 2_655 . . . ?
C5 C4 C6 C4 -6(14) 2_655 . . 2_655 ?
C5 C4 C6 C4 -9(21) . . . 2_655 ?
C5 C4 C6 C5 3(10) 2_655 . . . ?
C5 C4 C6 C6 -4(11) . . . 2_655 ?
C5 C4 C6 C6 -1(2) 2_655 . . 2_655 ?
C5 C4 C6 C7 3(6) 2_655 . . . ?
C5 C4 C6 C7 0(6) . . . . ?
C5 C4 C7 C3 176(6) . . . 2_655 ?
C5 C4 C7 C3 0(2) 2_655 . . 2_655 ?
C5 C4 C7 C3 -2(6) 2_655 . . . ?
C5 C4 C7 C3 174(8) . . . . ?
C5 C4 C7 C5 -176(5) 2_655 . . . ?
C5 C4 C7 C6 0(6) . . . . ?
C5 C4 C7 C6 -177(6) 2_655 . . . ?
C5 C4 C7 C7 175(6) . . . 2_655 ?
C5 C4 C7 C7 -0.9(17) 2_655 . . 2_655 ?
C5 C6 C7 C3 176(10) . . . 2_655 ?
C5 C6 C7 C3 173(13) . . . . ?
C5 C6 C7 C4 180(11) . . . . ?
C5 C6 C7 C7 175(10) . . . 2_655 ?
C6 C3 C5 C3 0(13) . . . 2_655 ?
C6 C3 C5 C4 0(5) . . . 2_655 ?
C6 C3 C5 C4 -1(4) . . . . ?
C6 C3 C5 C7 -172(15) . . . . ?
C6 C3 C7 C3 -8(23) . . . 2_655 ?
C6 C3 C7 C4 -2(3) . . . . ?
C6 C3 C7 C5 5(8) . . . . ?
C6 C3 C7 C7 -4(11) . . . 2_655 ?
C6 C4 C5 C3 1(5) 2_655 . . . ?
C6 C4 C5 C3 178(9) . . . . ?
C6 C4 C5 C3 178(9) . . . 2_655 ?
C6 C4 C5 C3 1(3) 2_655 . . 2_655 ?
C6 C4 C5 C4 173(16) . . . 2_655 ?
C6 C4 C5 C4 -3(7) 2_655 . . 2_655 ?
C6 C4 C5 C6 -176(9) 2_655 . . . ?
C6 C4 C5 C7 -180(11) . . . . ?
C6 C4 C5 C7 4(6) 2_655 . . . ?
C6 C4 C6 C3 2(6) 2_655 . . . ?
C6 C4 C6 C4 -5(11) 2_655 . . 2_655 ?
C6 C4 C6 C5 4(11) 2_655 . . . ?
C6 C4 C6 C7 4(7) 2_655 . . . ?
C6 C4 C7 C3 0(3) 2_655 . . 2_655 ?
C6 C4 C7 C3 -2(7) 2_655 . . . ?
C6 C4 C7 C3 176(6) . . . 2_655 ?
C6 C4 C7 C3 174(8) . . . . ?
C6 C4 C7 C5 -176(6) 2_655 . . . ?
C6 C4 C7 C5 0(6) . . . . ?
C6 C4 C7 C6 -176(6) 2_655 . . . ?
C6 C4 C7 C7 -1(2) 2_655 . . 2_655 ?
C6 C4 C7 C7 176(6) . . . 2_655 ?
C6 C5 C7 C3 -5(12) . . . 2_655 ?
C6 C5 C7 C3 -11(19) . . . . ?
C6 C5 C7 C4 0(6) . . . . ?
C6 C5 C7 C7 -5(11) . . . 2_655 ?
C6 C6 C7 C3 -1(3) 2_655 . . 2_655 ?
C6 C6 C7 C3 -4(8) 2_655 . . . ?
C6 C6 C7 C4 3(4) 2_655 . . . ?
C6 C6 C7 C5 -177(10) 2_655 . . . ?
C6 C6 C7 C7 -2(2) 2_655 . . 2_655 ?
C7 C3 C5 C3 -1(7) 2_655 . . 2_655 ?
C7 C3 C5 C3 171(21) . . . 2_655 ?
C7 C3 C5 C4 172(14) . . . 2_655 ?
C7 C3 C5 C4 0(4) 2_655 . . 2_655 ?
C7 C3 C5 C4 -2(6) 2_655 . . . ?
C7 C3 C5 C4 171(14) . . . . ?
C7 C3 C5 C6 -1(7) 2_655 . . . ?
C7 C3 C5 C6 172(15) . . . . ?
C7 C3 C5 C7 -173(15) 2_655 . . . ?
C7 C3 C6 C4 -3(6) 2_655 . . . ?
C7 C3 C6 C4 0(3) 2_655 . . 2_655 ?
C7 C3 C6 C4 176(8) . . . 2_655 ?
C7 C3 C6 C4 174(8) . . . . ?
C7 C3 C6 C5 -4(7) . . . . ?
C7 C3 C6 C5 179(7) 2_655 . . . ?
C7 C3 C6 C6 -1(2) 2_655 . . 2_655 ?
C7 C3 C6 C6 176(8) . . . 2_655 ?
C7 C3 C6 C7 -177(9) 2_655 . . . ?
C7 C3 C7 C3 -3(11) 2_655 . . 2_655 ?
C7 C3 C7 C4 2(9) 2_655 . . . ?
C7 C3 C7 C5 9(18) 2_655 . . . ?
C7 C3 C7 C6 4(11) 2_655 . . . ?
C7 C4 C5 C3 -3(4) . . . . ?
C7 C4 C5 C3 -3(5) . . . 2_655 ?
C7 C4 C5 C4 -7(12) . . . 2_655 ?
C7 C4 C5 C6 180(11) . . . . ?
C7 C4 C6 C3 -2(2) . . . . ?
C7 C4 C6 C4 -10(18) . . . 2_655 ?
C7 C4 C6 C5 0(6) . . . . ?
C7 C4 C6 C6 -4(7) . . . 2_655 ?
C7 C5 C6 C3 3(6) . . . . ?
C7 C5 C6 C4 4(11) . . . 2_655 ?
C7 C5 C6 C4 0(14) . . . . ?
C7 C5 C6 C6 3(10) . . . 2_655 ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 5.941
_oxdiff_exptl_absorpt_empirical_full_min 0.415
####################################################################### 
# 
# 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_immhypbbr4_358k
_database_code_depnum_ccdc_archive 'CCDC 2182361'
loop_
_audit_author_name
_audit_author_address
'Dawid Drozdowski'
;Institute of Low Temperature and Structure Research Polish Academy of Sciences
Poland
;
_audit_update_record             
;
2023-01-05 deposited with the CCDC.	2023-03-13 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT242_immhypbbr4_358k     
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        Pb1 Check
RESPONSE:  Bromines connected to Pb1 exhibit high thermal dynamics.
;
# Added during the CSD deposition process: Thursday 05 January 2023 10:17 AM
# end Validation Reply Form

_audit_creation_date             2022-12-22
_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, 0.5(C2 N4), C3 N2'
_chemical_formula_sum            'C4 Br4 N4 Pb'
_chemical_formula_weight         630.91
_chemical_melting_point          ?
_chemical_oxdiff_formula         PbBr4N4C4H12
_chemical_oxdiff_usercomment     'pomiar po schodzeniu i podgrzaniu'
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'
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           13
_space_group_name_H-M_alt        'P 1 2/c 1'
_space_group_name_Hall           '-P 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'

_cell_length_a                   6.0384(4)
_cell_length_b                   13.9702(9)
_cell_length_c                   8.5113(6)
_cell_angle_alpha                90
_cell_angle_beta                 92.062(7)
_cell_angle_gamma                90
_cell_volume                     717.53(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1590
_cell_measurement_temperature    358.00(10)
_cell_measurement_theta_max      24.3850
_cell_measurement_theta_min      3.3810
_shelx_estimated_absorpt_T_max   0.297
_shelx_estimated_absorpt_T_min   0.092
_exptl_absorpt_coefficient_mu    22.863
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.10551
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
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    2.920
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             548
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_av_unetI/netI     0.0399
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4566
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.361
_diffrn_reflns_theta_min         2.804
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      358.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6249
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -19.00  91.00   1.00   25.00    --   13.31  57.00-120.00  110
  2  ω    -23.00  49.00   1.00   25.00    --   13.31  77.00 -30.00   72
  3  ω    -17.00  74.00   1.00   25.00    --   13.31  35.00 178.38   91
;
_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      -0.1165913000
_diffrn_orient_matrix_UB_12      0.0043348000
_diffrn_orient_matrix_UB_13      -0.0111294000
_diffrn_orient_matrix_UB_21      -0.0122332000
_diffrn_orient_matrix_UB_22      -0.0033084000
_diffrn_orient_matrix_UB_23      0.0823941000
_diffrn_orient_matrix_UB_31      0.0092026000
_diffrn_orient_matrix_UB_32      0.0504581000
_diffrn_orient_matrix_UB_33      0.0063751000
_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                1198
_reflns_number_total             1480
_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 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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    ?
_refine_diff_density_max         1.890
_refine_diff_density_min         -1.556
_refine_diff_density_rms         0.201
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     59
_refine_ls_number_reflns         1480
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0443
_refine_ls_restrained_S_all      1.020
_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)+(0.0678P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1046
_refine_ls_wR_factor_ref         0.1145
_refine_special_details          ?
_olex2_refinement_description    
;
1. Shared sites
{C3, N3}
{C4, N4}
{C5, N5}
{C6, N6}
{C7, N7}
2. Restrained distances
 N2-N1 = N1-C1
 1.4 with sigma of 0.001
3. Restrained planarity
 C3, C4, C5, C6, C7, N3, N4, N5, N6, N7
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uiso(C1) = Uiso(N1) = Uiso(N2)
Uiso(C3) = Uiso(N3)
Uiso(C4) = Uiso(N4)
Uiso(C5) = Uiso(N5)
Uiso(C6) = Uiso(N6)
Uiso(C7) = Uiso(N7)
5. Others
 Fixed Sof: Br2(0.5) N1(0.5) C1(0.5) N2(0.5) C3(0.3) C4(0.3) C5(0.3) C6(0.3)
 C7(0.3) N3(0.2) N4(0.2) N5(0.2) N6(0.2) N7(0.2)
;
_atom_sites_solution_hydrogens   .
_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 0.000000 0.33960(3) 0.250000 0.0505(2) Uani 1 2 d S T P . .
Br1 Br 0.500000 0.33542(16) 0.250000 0.1193(9) Uani 1 2 d S T P . .
Br3 Br 0.0143(3) 0.19574(12) 0.49552(18) 0.1094(5) Uani 1 1 d . . . . .
Br2 Br -0.0395(15) 0.4877(6) 0.5201(9) 0.1299(17) Uani 0.5 1 d . . P . .
N1 N 0.482(5) 0.3914(17) 0.694(5) 0.225(17) Uiso 0.5 1 d D . P . .
C1 C 0.684(5) 0.347(3) 0.737(8) 0.225(17) Uiso 0.5 1 d D . P . .
N2 N 0.551(8) 0.2965(16) 0.674(5) 0.225(17) Uiso 0.5 1 d D . P . .
C3 C 0.434(5) 0.0730(19) 0.272(3) 0.094(10) Uiso 0.3 1 d . . P . .
C4 C 0.453(7) -0.0802(19) 0.270(5) 0.115(12) Uiso 0.3 1 d . . P . .
C5 C 0.327(7) -0.006(3) 0.314(4) 0.129(13) Uiso 0.3 1 d . . P . .
C6 C 0.371(7) -0.052(3) 0.299(4) 0.126(14) Uiso 0.3 1 d . . P . .
C7 C 0.374(7) 0.049(3) 0.291(3) 0.116(13) Uiso 0.3 1 d . . P . .
N3 N 0.434(5) 0.0730(19) 0.272(3) 0.094(10) Uiso 0.2 1 d . . P . .
N4 N 0.453(7) -0.0802(19) 0.270(5) 0.115(12) Uiso 0.2 1 d . . P . .
N5 N 0.327(7) -0.006(3) 0.314(4) 0.129(13) Uiso 0.2 1 d . . P . .
N6 N 0.371(7) -0.052(3) 0.299(4) 0.126(14) Uiso 0.2 1 d . . P . .
N7 N 0.374(7) 0.049(3) 0.291(3) 0.116(13) Uiso 0.2 1 d . . 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 Br1 3.0198(2) . ?
Pb1 Br1 3.0198(2) 1_455 ?
Pb1 Br3 2.8983(12) . ?
Pb1 Br3 2.8983(12) 2 ?
Pb1 Br2 3.108(7) . ?
Pb1 Br2 3.110(7) 3_566 ?
Pb1 Br2 3.108(7) 2 ?
Pb1 Br2 3.110(7) 4_565 ?
Br2 Br2 0.688(7) 3_566 ?
N1 N1 0.98(9) 2_656 ?
N1 C1 1.33(6) 2_656 ?
N1 C1 1.3999(11) . ?
N1 N2 1.4000(10) . ?
N1 N2 1.76(5) 2_656 ?
C1 N2 1.19(6) . ?
C1 N2 1.78(6) 2_656 ?
N2 N2 1.46(9) 2_656 ?
C3 C3 0.89(6) 2_655 ?
C3 C5 1.98(6) 2_655 ?
C3 C5 1.33(6) . ?
C3 C6 1.80(5) . ?
C3 C7 0.52(5) . ?
C3 C7 1.34(5) 2_655 ?
C4 C4 0.67(9) 2_655 ?
C4 C5 1.85(6) 2_655 ?
C4 C5 1.35(6) . ?
C4 C6 0.69(5) . ?
C4 C6 1.29(6) 2_655 ?
C4 C7 1.88(5) . ?
C5 C6 0.71(5) . ?
C5 C7 0.85(5) . ?
C6 C6 1.79(9) 2_655 ?
C6 C7 1.42(6) . ?
C7 C7 1.70(9) 2_655 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br1 Pb1 Br1 177.78(8) . 1_455 ?
Br1 Pb1 Br2 87.77(17) . 3_566 ?
Br1 Pb1 Br2 93.95(17) . 4_565 ?
Br1 Pb1 Br2 84.81(17) . 2 ?
Br1 Pb1 Br2 93.96(17) 1_455 3_566 ?
Br1 Pb1 Br2 96.67(17) 1_455 2 ?
Br1 Pb1 Br2 87.77(17) 1_455 4_565 ?
Br1 Pb1 Br2 96.67(17) . . ?
Br1 Pb1 Br2 84.81(17) 1_455 . ?
Br3 Pb1 Br1 89.45(5) 2 . ?
Br3 Pb1 Br1 89.01(5) 2 1_455 ?
Br3 Pb1 Br1 89.01(5) . . ?
Br3 Pb1 Br1 89.45(5) . 1_455 ?
Br3 Pb1 Br3 92.20(8) . 2 ?
Br3 Pb1 Br2 94.85(17) . 3_566 ?
Br3 Pb1 Br2 94.85(17) 2 4_565 ?
Br3 Pb1 Br2 85.96(17) 2 2 ?
Br3 Pb1 Br2 172.37(11) 2 3_566 ?
Br3 Pb1 Br2 173.57(13) . 2 ?
Br3 Pb1 Br2 173.57(13) 2 . ?
Br3 Pb1 Br2 85.96(17) . . ?
Br3 Pb1 Br2 172.37(11) . 4_565 ?
Br2 Pb1 Br2 12.71(13) . 3_566 ?
Br2 Pb1 Br2 86.72(4) 2 3_566 ?
Br2 Pb1 Br2 86.72(4) . 4_565 ?
Br2 Pb1 Br2 78.3(3) 3_566 4_565 ?
Br2 Pb1 Br2 12.71(13) 2 4_565 ?
Br2 Pb1 Br2 96.5(3) 2 . ?
Pb1 Br1 Pb1 177.78(8) 1_655 . ?
Pb1 Br2 Pb1 167.29(13) . 3_566 ?
Br2 Br2 Pb1 83.5(12) 3_566 3_566 ?
Br2 Br2 Pb1 83.8(12) 3_566 . ?
N1 N1 C1 73(4) 2_656 2_656 ?
N1 N1 C1 65(3) 2_656 . ?
N1 N1 N2 53(2) 2_656 2_656 ?
N1 N1 N2 94(2) 2_656 . ?
C1 N1 C1 110(4) 2_656 . ?
C1 N1 N2 68(3) . 2_656 ?
C1 N1 N2 81(3) 2_656 . ?
C1 N1 N2 42(2) 2_656 2_656 ?
C1 N1 N2 50(3) . . ?
N2 N1 N2 54(3) . 2_656 ?
N1 C1 N1 42(4) 2_656 . ?
N1 C1 N2 66(3) . 2_656 ?
N1 C1 N2 51.0(19) 2_656 2_656 ?
N2 C1 N1 88(3) . 2_656 ?
N2 C1 N1 65.0(13) . . ?
N2 C1 N2 54(4) . 2_656 ?
N1 N2 N1 34(3) . 2_656 ?
N1 N2 C1 48(2) . 2_656 ?
N1 N2 C1 46.6(11) 2_656 2_656 ?
N1 N2 N2 76(3) . 2_656 ?
C1 N2 N1 49(3) . 2_656 ?
C1 N2 N1 65.0(13) . . ?
C1 N2 C1 96(3) . 2_656 ?
C1 N2 N2 84(5) . 2_656 ?
N2 N2 N1 50.6(18) 2_656 2_656 ?
N2 N2 C1 41(3) 2_656 2_656 ?
C3 C3 C5 33.9(15) 2_655 2_655 ?
C3 C3 C5 124(2) 2_655 . ?
C3 C3 C6 104.4(18) 2_655 . ?
C3 C3 C7 14(2) 2_655 2_655 ?
C5 C3 C5 90(3) . 2_655 ?
C5 C3 C6 20(2) . . ?
C5 C3 C7 110(4) . 2_655 ?
C6 C3 C5 71(2) . 2_655 ?
C7 C3 C3 141(7) . 2_655 ?
C7 C3 C5 107(7) . 2_655 ?
C7 C3 C5 20(2) 2_655 2_655 ?
C7 C3 C5 17(7) . . ?
C7 C3 C6 90(3) 2_655 . ?
C7 C3 C6 37(7) . . ?
C7 C3 C7 127(9) . 2_655 ?
C4 C4 C5 130(2) 2_655 . ?
C4 C4 C5 34.3(17) 2_655 2_655 ?
C4 C4 C6 145(6) 2_655 . ?
C4 C4 C6 18(2) 2_655 2_655 ?
C4 C4 C7 105.8(19) 2_655 . ?
C5 C4 C5 95(3) . 2_655 ?
C5 C4 C7 72(2) 2_655 . ?
C5 C4 C7 24(2) . . ?
C6 C4 C5 16(3) 2_655 2_655 ?
C6 C4 C5 112(4) 2_655 . ?
C6 C4 C5 15(6) . . ?
C6 C4 C5 111(6) . 2_655 ?
C6 C4 C6 127(8) . 2_655 ?
C6 C4 C7 39(5) . . ?
C6 C4 C7 88(3) 2_655 . ?
C3 C5 C3 22.0(18) . 2_655 ?
C3 C5 C4 106(3) . . ?
C3 C5 C4 90(3) . 2_655 ?
C4 C5 C3 68.1(19) 2_655 2_655 ?
C4 C5 C3 84(3) . 2_655 ?
C4 C5 C4 16(2) . 2_655 ?
C6 C5 C3 121(7) . . ?
C6 C5 C3 99(6) . 2_655 ?
C6 C5 C4 15(6) . . ?
C6 C5 C4 31(5) . 2_655 ?
C6 C5 C7 131(9) . . ?
C7 C5 C3 32(4) . 2_655 ?
C7 C5 C3 10(4) . . ?
C7 C5 C4 116(6) . . ?
C7 C5 C4 100(5) . 2_655 ?
C4 C6 C3 111(6) . . ?
C4 C6 C3 93(3) 2_655 . ?
C4 C6 C4 17(4) . 2_655 ?
C4 C6 C5 150(10) . . ?
C4 C6 C6 18(2) 2_655 2_655 ?
C4 C6 C6 35(6) . 2_655 ?
C4 C6 C7 123(7) . . ?
C4 C6 C7 106(4) 2_655 . ?
C5 C6 C3 39(5) . . ?
C5 C6 C4 133(8) . 2_655 ?
C5 C6 C6 115(6) . 2_655 ?
C5 C6 C7 27(5) . . ?
C6 C6 C3 75.6(17) 2_655 . ?
C7 C6 C3 13(2) . . ?
C7 C6 C6 88(3) . 2_655 ?
C3 C7 C3 25(5) . 2_655 ?
C3 C7 C4 88(3) 2_655 . ?
C3 C7 C4 113(8) . . ?
C3 C7 C5 153(10) . . ?
C3 C7 C6 131(8) . . ?
C3 C7 C6 106(4) 2_655 . ?
C3 C7 C7 14(2) 2_655 2_655 ?
C3 C7 C7 39(7) . 2_655 ?
C5 C7 C3 128(6) . 2_655 ?
C5 C7 C4 40(4) . . ?
C5 C7 C6 22(4) . . ?
C5 C7 C7 114(5) . 2_655 ?
C6 C7 C4 18(3) . . ?
C6 C7 C7 92(2) . 2_655 ?
C7 C7 C4 74.0(18) 2_655 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 N1 C1 N2 118(4) 2_656 . . . ?
N1 N1 C1 N2 58(2) 2_656 . . 2_656 ?
N1 N1 N2 C1 -53(4) 2_656 . . . ?
N1 N1 N2 C1 72(4) 2_656 . . 2_656 ?
N1 N1 N2 N2 37(5) 2_656 . . 2_656 ?
N1 C1 N2 N1 36(4) 2_656 . . . ?
N1 C1 N2 N1 -36(4) . . . 2_656 ?
N1 C1 N2 C1 -37(3) . . . 2_656 ?
N1 C1 N2 C1 -1(3) 2_656 . . 2_656 ?
N1 C1 N2 N2 -41(3) 2_656 . . 2_656 ?
N1 C1 N2 N2 -77(4) . . . 2_656 ?
C1 N1 C1 N1 -59(4) 2_656 . . 2_656 ?
C1 N1 C1 N2 59(3) 2_656 . . . ?
C1 N1 C1 N2 -1(3) 2_656 . . 2_656 ?
C1 N1 N2 N1 -72(4) 2_656 . . 2_656 ?
C1 N1 N2 N1 53(4) . . . 2_656 ?
C1 N1 N2 C1 -125(4) 2_656 . . . ?
C1 N1 N2 C1 125(4) . . . 2_656 ?
C1 N1 N2 N2 90(5) . . . 2_656 ?
C1 N1 N2 N2 -35(4) 2_656 . . 2_656 ?
N2 N1 C1 N1 -58(2) 2_656 . . 2_656 ?
N2 N1 C1 N1 -118(4) . . . 2_656 ?
N2 N1 C1 N2 -60(4) . . . 2_656 ?
N2 N1 C1 N2 60(4) 2_656 . . . ?
N2 N1 N2 N1 -37(5) 2_656 . . 2_656 ?
N2 N1 N2 C1 -90(5) 2_656 . . . ?
N2 N1 N2 C1 35(4) 2_656 . . 2_656 ?
N2 C1 N2 N1 77(4) 2_656 . . . ?
N2 C1 N2 N1 41(3) 2_656 . . 2_656 ?
N2 C1 N2 C1 40(3) 2_656 . . 2_656 ?
C3 C3 C5 C4 -2(7) 2_655 . . . ?
C3 C3 C5 C4 -3(6) 2_655 . . 2_655 ?
C3 C3 C5 C6 -3(8) 2_655 . . . ?
C3 C3 C5 C7 -171(17) 2_655 . . . ?
C3 C3 C6 C4 -3(4) 2_655 . . 2_655 ?
C3 C3 C6 C4 -1(7) 2_655 . . . ?
C3 C3 C6 C5 178(7) 2_655 . . . ?
C3 C3 C6 C6 -2(4) 2_655 . . 2_655 ?
C3 C3 C6 C7 -176(10) 2_655 . . . ?
C3 C3 C7 C4 4(14) 2_655 . . . ?
C3 C3 C7 C5 12(23) 2_655 . . . ?
C3 C3 C7 C6 6(16) 2_655 . . . ?
C3 C3 C7 C7 1(7) 2_655 . . 2_655 ?
C3 C5 C6 C3 -1(3) 2_655 . . . ?
C3 C5 C6 C4 1(12) 2_655 . . . ?
C3 C5 C6 C4 -1(7) . . . 2_655 ?
C3 C5 C6 C4 2(13) . . . . ?
C3 C5 C6 C4 -2(6) 2_655 . . 2_655 ?
C3 C5 C6 C6 -1(4) 2_655 . . 2_655 ?
C3 C5 C6 C6 0(6) . . . 2_655 ?
C3 C5 C6 C7 -4(4) 2_655 . . . ?
C3 C5 C6 C7 -3(3) . . . . ?
C3 C5 C7 C3 7(12) . . . 2_655 ?
C3 C5 C7 C3 -7(12) 2_655 . . . ?
C3 C5 C7 C4 6(6) 2_655 . . . ?
C3 C5 C7 C4 13(15) . . . . ?
C3 C5 C7 C6 7(8) 2_655 . . . ?
C3 C5 C7 C6 14(16) . . . . ?
C3 C5 C7 C7 1.0(18) 2_655 . . 2_655 ?
C3 C5 C7 C7 8(11) . . . 2_655 ?
C3 C6 C7 C3 2(7) . . . 2_655 ?
C3 C6 C7 C4 6(9) . . . . ?
C3 C6 C7 C5 -172(10) . . . . ?
C3 C6 C7 C7 3(6) . . . 2_655 ?
C4 C4 C5 C3 -5(10) 2_655 . . 2_655 ?
C4 C4 C5 C3 -4(12) 2_655 . . . ?
C4 C4 C5 C6 174(19) 2_655 . . . ?
C4 C4 C5 C7 -2(12) 2_655 . . . ?
C4 C4 C6 C3 -7(19) 2_655 . . . ?
C4 C4 C6 C5 -8(26) 2_655 . . . ?
C4 C4 C6 C6 -5(12) 2_655 . . 2_655 ?
C4 C4 C6 C7 -5(20) 2_655 . . . ?
C4 C4 C7 C3 -8(10) 2_655 . . . ?
C4 C4 C7 C3 -6(7) 2_655 . . 2_655 ?
C4 C4 C7 C5 179(10) 2_655 . . . ?
C4 C4 C7 C6 177(12) 2_655 . . . ?
C4 C4 C7 C7 -6(7) 2_655 . . 2_655 ?
C4 C5 C6 C3 -2(13) . . . . ?
C4 C5 C6 C3 1(7) 2_655 . . . ?
C4 C5 C6 C4 -3(11) . . . 2_655 ?
C4 C5 C6 C4 3(11) 2_655 . . . ?
C4 C5 C6 C6 1(3) 2_655 . . 2_655 ?
C4 C5 C6 C6 -2(9) . . . 2_655 ?
C4 C5 C6 C7 -5(15) . . . . ?
C4 C5 C6 C7 -2(9) 2_655 . . . ?
C4 C5 C7 C3 -13(14) 2_655 . . . ?
C4 C5 C7 C3 -6(6) . . . 2_655 ?
C4 C5 C7 C3 -13(15) . . . . ?
C4 C5 C7 C3 -6(4) 2_655 . . 2_655 ?
C4 C5 C7 C4 -1(3) 2_655 . . . ?
C4 C5 C7 C6 1(5) 2_655 . . . ?
C4 C5 C7 C6 1(4) . . . . ?
C4 C5 C7 C7 -5(5) . . . 2_655 ?
C4 C5 C7 C7 -5(4) 2_655 . . 2_655 ?
C4 C6 C7 C3 -5(3) 2_655 . . 2_655 ?
C4 C6 C7 C3 -7(8) 2_655 . . . ?
C4 C6 C7 C3 -6(9) . . . . ?
C4 C6 C7 C3 -3(6) . . . 2_655 ?
C4 C6 C7 C4 -2(6) 2_655 . . . ?
C4 C6 C7 C5 -179(7) 2_655 . . . ?
C4 C6 C7 C5 -177(9) . . . . ?
C4 C6 C7 C7 -3(6) . . . 2_655 ?
C4 C6 C7 C7 -4(3) 2_655 . . 2_655 ?
C5 C3 C5 C3 2(5) 2_655 . . 2_655 ?
C5 C3 C5 C4 -1.0(14) 2_655 . . 2_655 ?
C5 C3 C5 C4 0(3) 2_655 . . . ?
C5 C3 C5 C6 0(4) 2_655 . . . ?
C5 C3 C5 C7 -168(14) 2_655 . . . ?
C5 C3 C6 C4 179(6) . . . 2_655 ?
C5 C3 C6 C4 1(5) 2_655 . . . ?
C5 C3 C6 C4 -1(2) 2_655 . . 2_655 ?
C5 C3 C6 C4 -179(7) . . . . ?
C5 C3 C6 C5 180(4) 2_655 . . . ?
C5 C3 C6 C6 -0.4(15) 2_655 . . 2_655 ?
C5 C3 C6 C6 180(5) . . . 2_655 ?
C5 C3 C6 C7 -174(7) 2_655 . . . ?
C5 C3 C6 C7 6(7) . . . . ?
C5 C3 C7 C3 -12(23) . . . 2_655 ?
C5 C3 C7 C3 0(9) 2_655 . . 2_655 ?
C5 C3 C7 C4 -9(11) . . . . ?
C5 C3 C7 C4 4(5) 2_655 . . . ?
C5 C3 C7 C5 12(15) 2_655 . . . ?
C5 C3 C7 C6 -7(9) . . . . ?
C5 C3 C7 C6 5(7) 2_655 . . . ?
C5 C3 C7 C7 1(2) 2_655 . . 2_655 ?
C5 C3 C7 C7 -11(16) . . . 2_655 ?
C5 C4 C5 C3 -1.0(14) 2_655 . . 2_655 ?
C5 C4 C5 C3 0(3) 2_655 . . . ?
C5 C4 C5 C4 4(9) 2_655 . . 2_655 ?
C5 C4 C5 C6 178(13) 2_655 . . . ?
C5 C4 C5 C7 2(4) 2_655 . . . ?
C5 C4 C6 C3 1(9) . . . . ?
C5 C4 C6 C3 -1(5) 2_655 . . . ?
C5 C4 C6 C4 6(15) 2_655 . . 2_655 ?
C5 C4 C6 C4 8(26) . . . 2_655 ?
C5 C4 C6 C5 -2(13) 2_655 . . . ?
C5 C4 C6 C6 1(2) 2_655 . . 2_655 ?
C5 C4 C6 C6 3(14) . . . 2_655 ?
C5 C4 C6 C7 3(8) . . . . ?
C5 C4 C6 C7 1(6) 2_655 . . . ?
C5 C4 C7 C3 -2.4(17) 2_655 . . 2_655 ?
C5 C4 C7 C3 175(5) . . . 2_655 ?
C5 C4 C7 C3 -4(6) 2_655 . . . ?
C5 C4 C7 C3 174(7) . . . . ?
C5 C4 C7 C5 -178(4) 2_655 . . . ?
C5 C4 C7 C6 -179(6) 2_655 . . . ?
C5 C4 C7 C6 -2(5) . . . . ?
C5 C4 C7 C7 -2.4(16) 2_655 . . 2_655 ?
C5 C4 C7 C7 175(5) . . . 2_655 ?
C5 C6 C7 C3 174(7) . . . 2_655 ?
C5 C6 C7 C3 172(10) . . . . ?
C5 C6 C7 C4 177(9) . . . . ?
C5 C6 C7 C7 174(7) . . . 2_655 ?
C6 C3 C5 C3 3(8) . . . 2_655 ?
C6 C3 C5 C4 -1(4) . . . 2_655 ?
C6 C3 C5 C4 1(4) . . . . ?
C6 C3 C5 C7 -168(15) . . . . ?
C6 C3 C7 C3 -6(16) . . . 2_655 ?
C6 C3 C7 C4 -2(3) . . . . ?
C6 C3 C7 C5 7(9) . . . . ?
C6 C3 C7 C7 -4(9) . . . 2_655 ?
C6 C4 C5 C3 -1(4) 2_655 . . . ?
C6 C4 C5 C3 -178(12) . . . . ?
C6 C4 C5 C3 -179(12) . . . 2_655 ?
C6 C4 C5 C3 -2(3) 2_655 . . 2_655 ?
C6 C4 C5 C4 -174(19) . . . 2_655 ?
C6 C4 C5 C4 3(8) 2_655 . . 2_655 ?
C6 C4 C5 C6 177(12) 2_655 . . . ?
C6 C4 C5 C7 -176(12) . . . . ?
C6 C4 C5 C7 1(5) 2_655 . . . ?
C6 C4 C6 C3 -2(7) 2_655 . . . ?
C6 C4 C6 C4 5(12) 2_655 . . 2_655 ?
C6 C4 C6 C5 -3(14) 2_655 . . . ?
C6 C4 C6 C7 0(8) 2_655 . . . ?
C6 C4 C7 C3 177(6) . . . 2_655 ?
C6 C4 C7 C3 -3(2) 2_655 . . 2_655 ?
C6 C4 C7 C3 175(8) . . . . ?
C6 C4 C7 C3 -5(6) 2_655 . . . ?
C6 C4 C7 C5 2(5) . . . . ?
C6 C4 C7 C5 -179(5) 2_655 . . . ?
C6 C4 C7 C6 180(6) 2_655 . . . ?
C6 C4 C7 C7 -3(2) 2_655 . . 2_655 ?
C6 C4 C7 C7 177(6) . . . 2_655 ?
C6 C5 C7 C3 -7(8) . . . 2_655 ?
C6 C5 C7 C3 -14(16) . . . . ?
C6 C5 C7 C4 -1(4) . . . . ?
C6 C5 C7 C7 -6(7) . . . 2_655 ?
C6 C6 C7 C3 -6(7) 2_655 . . . ?
C6 C6 C7 C3 -3(2) 2_655 . . 2_655 ?
C6 C6 C7 C4 0(4) 2_655 . . . ?
C6 C6 C7 C5 -177(7) 2_655 . . . ?
C6 C6 C7 C7 -3(2) 2_655 . . 2_655 ?
C7 C3 C5 C3 171(17) . . . 2_655 ?
C7 C3 C5 C3 0(4) 2_655 . . 2_655 ?
C7 C3 C5 C4 -3(2) 2_655 . . 2_655 ?
C7 C3 C5 C4 168(14) . . . . ?
C7 C3 C5 C4 167(14) . . . 2_655 ?
C7 C3 C5 C4 -2(4) 2_655 . . . ?
C7 C3 C5 C6 168(15) . . . . ?
C7 C3 C5 C6 -3(5) 2_655 . . . ?
C7 C3 C5 C7 -171(14) 2_655 . . . ?
C7 C3 C6 C4 -2(5) 2_655 . . . ?
C7 C3 C6 C4 -4(2) 2_655 . . 2_655 ?
C7 C3 C6 C4 175(8) . . . . ?
C7 C3 C6 C4 173(8) . . . 2_655 ?
C7 C3 C6 C5 177(5) 2_655 . . . ?
C7 C3 C6 C5 -6(7) . . . . ?
C7 C3 C6 C6 -2.6(19) 2_655 . . 2_655 ?
C7 C3 C6 C6 174(7) . . . 2_655 ?
C7 C3 C6 C7 -177(7) 2_655 . . . ?
C7 C3 C7 C3 -1(7) 2_655 . . 2_655 ?
C7 C3 C7 C4 2(7) 2_655 . . . ?
C7 C3 C7 C5 11(16) 2_655 . . . ?
C7 C3 C7 C6 4(9) 2_655 . . . ?
C7 C4 C5 C3 -3(3) . . . 2_655 ?
C7 C4 C5 C3 -2(3) . . . . ?
C7 C4 C5 C4 2(12) . . . 2_655 ?
C7 C4 C5 C6 176(12) . . . . ?
C7 C4 C6 C3 -1(2) . . . . ?
C7 C4 C6 C4 5(20) . . . 2_655 ?
C7 C4 C6 C5 -3(8) . . . . ?
C7 C4 C6 C6 0(8) . . . 2_655 ?
C7 C5 C6 C3 3(3) . . . . ?
C7 C5 C6 C4 5(15) . . . . ?
C7 C5 C6 C4 2(9) . . . 2_655 ?
C7 C5 C6 C6 3(8) . . . 2_655 ?

_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 3.328
_oxdiff_exptl_absorpt_empirical_full_min 0.372
####################################################################### 
# 
# 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_immhypbcl4_295k
_database_code_depnum_ccdc_archive 'CCDC 2182519'
loop_
_audit_author_name
_audit_author_address
'Dawid Drozdowski'
;Institute of Low Temperature and Structure Research Polish Academy of Sciences
Poland
;
_audit_update_record             
;
2023-01-12 deposited with the CCDC.	2023-03-13 downloaded from the CCDC.
;
_audit_creation_date             2023-01-10
_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         'Cl4 Pb, C3 H5 N2, C H5 N1.333, 0.667(N)'
_chemical_formula_sum            'C4 H10 Cl4 N4 Pb'
_chemical_formula_weight         463.15
_chemical_melting_point          ?
_chemical_oxdiff_formula         PbCl4C4N4
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   5.7168(2)
_cell_length_b                   27.8826(10)
_cell_length_c                   8.0079(3)
_cell_angle_alpha                90
_cell_angle_beta                 90.132(3)
_cell_angle_gamma                90
_cell_volume                     1276.45(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    10071
_cell_measurement_temperature    294.99(10)
_cell_measurement_theta_max      28.6400
_cell_measurement_theta_min      3.3060
_shelx_estimated_absorpt_T_max   0.767
_shelx_estimated_absorpt_T_min   0.228
_exptl_absorpt_coefficient_mu    14.021
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36236
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    2.410
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_unetI/netI     0.0198
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            25547
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.646
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      294.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6249
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.995
_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    -23.00  97.00   1.00   12.00    --   13.31  77.00  30.00  120
  2  ω    -23.00  97.00   1.00   12.00    --   13.31  77.00-120.00  120
  3  ω    -23.00  97.00   1.00   12.00    --   13.31  77.00  90.00  120
  4  ω    -50.00  70.00   1.00   12.00    --  -14.40  77.00  90.00  120
  5  ω     35.00 106.00   1.00   12.00    --   13.31 178.00 -60.00   71
  6  ω     32.00 104.00   1.00   12.00    --   13.31-178.00 120.00   72
  7  ω    -18.00  93.00   1.00   12.00    --   13.31  37.00-150.00  111
  8  ω    -92.00 -39.00   1.00   12.00    --  -14.40 154.00 152.00   53
  9  ω   -105.00 -32.00   1.00   12.00    --  -14.40 178.00-150.00   73
;
_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      0.0011755000
_diffrn_orient_matrix_UB_12      0.0172150000
_diffrn_orient_matrix_UB_13      0.0652082000
_diffrn_orient_matrix_UB_21      -0.0192520000
_diffrn_orient_matrix_UB_22      -0.0184795000
_diffrn_orient_matrix_UB_23      0.0592863000
_diffrn_orient_matrix_UB_31      0.1225466000
_diffrn_orient_matrix_UB_32      -0.0030599000
_diffrn_orient_matrix_UB_33      0.0089054000
_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                2380
_reflns_number_total             2585
_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 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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         1.235
_refine_diff_density_min         -2.039
_refine_diff_density_rms         0.134
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.242
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     114
_refine_ls_number_reflns         2585
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0288
_refine_ls_restrained_S_all      1.242
_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)+(0.0145P)²+6.5891P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0605
_refine_ls_wR_factor_ref         0.0616
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N7A) = Uanis(N6) = Uanis(C8) = Uanis(N7C) = Uanis(N7B)
3. Others
 Fixed Sof: N7A(0.33333) N7C(0.33333) N7B(0.33333)
4.a Rotating group:
 N6(H6A,H6B)
4.b Aromatic/amide H refined with riding coordinates:
 N4(H4), C3(H3), N1(H1), C2(H2), C5(H5)
4.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C)
;
_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 0.47655(4) 0.17380(2) 0.68180(3) 0.02832(8) Uani 1 1 d . . . . .
Cl1 Cl 0.4640(4) 0.11432(7) 0.9774(2) 0.0533(5) Uani 1 1 d . . . . .
Cl2 Cl 0.4733(3) 0.09450(7) 0.4859(2) 0.0503(5) Uani 1 1 d . . . . .
Cl3 Cl 0.4737(4) 0.22885(8) 0.3817(3) 0.0614(6) Uani 1 1 d . . . . .
Cl4 Cl -0.0212(3) 0.16262(8) 0.6821(3) 0.0622(6) Uani 1 1 d . . . . .
N4 N -0.0634(15) -0.0389(3) 0.2875(10) 0.073(2) Uani 1 1 d . . . . .
H4 H -0.122674 -0.066161 0.314654 0.087 Uiso 1 1 calc R U . . .
C3 C 0.1428(17) -0.0325(3) 0.2086(11) 0.062(2) Uani 1 1 d . . . . .
H3 H 0.247195 -0.056187 0.175173 0.074 Uiso 1 1 calc R U . . .
N1 N -0.0189(17) 0.0355(3) 0.2559(11) 0.073(2) Uani 1 1 d . . . . .
H1 H -0.043492 0.065897 0.259632 0.087 Uiso 1 1 calc R U . . .
C2 C 0.1663(18) 0.0145(4) 0.1886(12) 0.071(3) Uani 1 1 d . . . . .
H2 H 0.290452 0.030017 0.136606 0.086 Uiso 1 1 calc R U . . .
C5 C -0.1578(19) 0.0027(4) 0.3157(13) 0.078(3) Uani 1 1 d . . . . .
H5 H -0.299626 0.008157 0.369103 0.094 Uiso 1 1 calc R U . . .
N6 N -0.0406(18) 0.1372(3) 0.2586(11) 0.0821(19) Uani 1 1 d . . . . .
H6A H 0.088903 0.143570 0.316412 0.098 Uiso 1 1 d R U . . .
H6B H -0.164458 0.147969 0.314391 0.098 Uiso 1 1 d R U . . .
C8 C -0.023(2) 0.2117(3) 0.1066(13) 0.0821(19) Uani 1 1 d . . . . .
H8A H -0.152972 0.224800 0.045549 0.123 Uiso 1 1 calc R U . . .
H8B H 0.120411 0.223587 0.060710 0.123 Uiso 1 1 calc R U . . .
H8C H -0.034432 0.220943 0.221763 0.123 Uiso 1 1 calc R U . . .
N7A N 0.075(6) 0.1678(9) 0.182(4) 0.0821(19) Uani 0.3333 1 d . . P . .
N7C N -0.124(6) 0.1668(10) 0.161(4) 0.0821(19) Uani 0.3333 1 d . . P . .
N7B N -0.027(6) 0.1608(10) 0.094(4) 0.0821(19) Uani 0.3333 1 d . . 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 Cl1 2.8911(19) . ?
Pb1 Cl2 2.7113(18) . ?
Pb1 Cl3 2.852(2) . ?
Pb1 Cl3 3.151(2) 4_566 ?
Pb1 Cl4 2.8625(18) . ?
Pb1 Cl4 2.8882(18) 1_655 ?
N4 H4 0.8600 . ?
N4 C3 1.350(12) . ?
N4 C5 1.301(12) . ?
C3 H3 0.9300 . ?
C3 C2 1.328(13) . ?
N1 H1 0.8600 . ?
N1 C2 1.325(12) . ?
N1 C5 1.302(13) . ?
C2 H2 0.9300 . ?
C5 H5 0.9300 . ?
N6 H6A 0.8900 . ?
N6 H6B 0.8900 . ?
N6 N7B 1.47(3) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C8 N7B 1.42(3) . ?
N7A H6A 1.2745 . ?
N7C H6B 1.3557 . ?

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
Cl1 Pb1 Cl3 94.48(6) . 4_566 ?
Cl2 Pb1 Cl1 90.33(6) . . ?
Cl2 Pb1 Cl3 87.21(7) . . ?
Cl2 Pb1 Cl3 175.12(6) . 4_566 ?
Cl2 Pb1 Cl4 84.61(6) . . ?
Cl2 Pb1 Cl4 85.30(6) . 1_655 ?
Cl3 Pb1 Cl1 176.98(6) . . ?
Cl3 Pb1 Cl3 87.96(2) . 4_566 ?
Cl3 Pb1 Cl4 93.19(7) . . ?
Cl3 Pb1 Cl4 93.58(7) . 1_655 ?
Cl4 Pb1 Cl1 84.85(7) . . ?
Cl4 Pb1 Cl1 87.94(7) 1_655 . ?
Cl4 Pb1 Cl3 95.67(6) 1_655 4_566 ?
Cl4 Pb1 Cl3 95.00(6) . 4_566 ?
Cl4 Pb1 Cl4 167.55(9) . 1_655 ?
Pb1 Cl4 Pb1 167.55(9) . 1_455 ?
C3 N4 H4 125.5 . . ?
C5 N4 H4 125.5 . . ?
C5 N4 C3 109.0(8) . . ?
N4 C3 H3 127.0 . . ?
C2 C3 N4 106.0(8) . . ?
C2 C3 H3 127.0 . . ?
C2 N1 H1 125.4 . . ?
C5 N1 H1 125.4 . . ?
C5 N1 C2 109.2(8) . . ?
C3 C2 H2 126.1 . . ?
N1 C2 C3 107.8(9) . . ?
N1 C2 H2 126.1 . . ?
N4 C5 N1 108.0(9) . . ?
N4 C5 H5 126.0 . . ?
N1 C5 H5 126.0 . . ?
H6A N6 H6B 109.5 . . ?
N7B N6 H6A 109.4 . . ?
N7B N6 H6B 109.9 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N7B C8 H8A 109.5 . . ?
N7B C8 H8B 109.5 . . ?
N7B C8 H8C 109.5 . . ?
C8 N7B N6 113(2) . . ?

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
N4 H4 Cl2 0.86 2.68 3.348(8) 134.9 3_556 yes
N4 H4 Cl4 0.86 2.81 3.491(8) 137.0 3_556 yes
C3 H3 Cl1 0.93 2.62 3.534(9) 168.5 3_656 yes
N1 H1 N6 0.86 1.99 2.840(11) 169.9 . 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
N4 C3 C2 N1 0.9(11) . . . . ?
C3 N4 C5 N1 0.5(12) . . . . ?
C2 N1 C5 N4 0.1(12) . . . . ?
C5 N4 C3 C2 -0.9(11) . . . . ?
C5 N1 C2 C3 -0.7(12) . . . . ?

_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 2.000
_oxdiff_exptl_absorpt_empirical_full_min 0.620
####################################################################### 
# 
# 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_immhypbcl4_100k
_database_code_depnum_ccdc_archive 'CCDC 2235385'
loop_
_audit_author_name
_audit_author_address
'Dawid Drozdowski'
;Institute of Low Temperature and Structure Research Polish Academy of Sciences
Poland
;
_audit_update_record             
;
2023-01-12 deposited with the CCDC.	2023-03-13 downloaded from the CCDC.
;
_audit_creation_date             2023-01-10
_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         'Cl4 Pb, C3 H5 N2, C H7 N2'
_chemical_formula_sum            'C4 H12 Cl4 N4 Pb'
_chemical_formula_weight         465.17
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Pb Cl4 C4 N4'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   5.6652(2)
_cell_length_b                   27.3877(17)
_cell_length_c                   7.9492(4)
_cell_angle_alpha                90
_cell_angle_beta                 90.453(4)
_cell_angle_gamma                90
_cell_volume                     1233.33(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6735
_cell_measurement_temperature    100.00(12)
_cell_measurement_theta_max      29.0680
_cell_measurement_theta_min      2.9930
_shelx_estimated_absorpt_T_max   0.594
_shelx_estimated_absorpt_T_min   0.128
_exptl_absorpt_coefficient_mu    14.512
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.20069
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
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    2.505
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            13157
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.368
_diffrn_reflns_theta_min         2.668
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(12)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6249
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_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    -78.00 -32.00   1.00    7.00    --   13.31 178.00 150.00   46
  2  ω    -19.00  91.00   1.00    7.00    --   13.31  57.00-180.00  110
  3  ω    -71.00  49.00   1.00    7.00    --   13.31 -77.00  60.00  120
  4  ω    -94.00 -15.00   1.00    7.00    --  -14.40 -37.00 -90.00   79
  5  ω    -46.00  65.00   1.00    7.00    --  -14.40  37.00-120.00  111
;
_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      -0.1084826000
_diffrn_orient_matrix_UB_12      -0.0104358000
_diffrn_orient_matrix_UB_13      -0.0270737000
_diffrn_orient_matrix_UB_21      0.0598084000
_diffrn_orient_matrix_UB_22      -0.0217871000
_diffrn_orient_matrix_UB_23      -0.0221390000
_diffrn_orient_matrix_UB_31      -0.0184731000
_diffrn_orient_matrix_UB_32      -0.0092946000
_diffrn_orient_matrix_UB_33      0.0820984000
_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                2351
_reflns_number_total             2508
_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 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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         1.295
_refine_diff_density_min         -1.779
_refine_diff_density_rms         0.217
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         2508
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0288
_refine_ls_restrained_S_all      1.157
_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)+(0.0344P)²+4.5879P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0700
_refine_ls_wR_factor_ref         0.0714
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Rotating group:
 N6(H6A,H6B)
2.b Secondary CH2 refined with riding coordinates:
 N7B(H7BA,H7BB)
2.c Aromatic/amide H refined with riding coordinates:
 C4(H4), N3(H3), N1(H1), C2(H2), C5(H5)
2.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C)
;
_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 0.45167(3) 0.17465(2) 0.66240(3) 0.00947(9) Uani 1 1 d . . . . .
Cl1 Cl 0.4551(2) 0.12020(6) 0.97325(17) 0.0161(3) Uani 1 1 d . . . . .
Cl2 Cl 0.4569(2) 0.09103(6) 0.48847(17) 0.0154(3) Uani 1 1 d . . . . .
Cl3 Cl 0.4004(3) 0.22231(6) 0.34756(18) 0.0187(3) Uani 1 1 d . . . . .
Cl4 Cl -0.0332(2) 0.15800(6) 0.67769(18) 0.0162(3) Uani 1 1 d . . . . .
C4 C -0.1569(12) 0.0050(3) 0.3169(8) 0.0224(15) Uani 1 1 d . . . . .
H4 H -0.303811 0.009979 0.371076 0.027 Uiso 1 1 calc R U . . .
N3 N -0.0534(9) -0.0379(2) 0.2920(6) 0.0189(12) Uani 1 1 d . . . . .
H3 H -0.109922 -0.066379 0.322891 0.023 Uiso 1 1 calc R U . . .
N1 N -0.0227(9) 0.0392(2) 0.2545(6) 0.0196(12) Uani 1 1 d . . . . .
H1 H -0.053299 0.070701 0.256350 0.023 Uiso 1 1 calc R U . . .
C2 C 0.1552(11) -0.0305(3) 0.2107(8) 0.0203(14) Uani 1 1 d . . . . .
H2 H 0.265456 -0.054763 0.178129 0.024 Uiso 1 1 calc R U . . .
C5 C 0.1736(11) 0.0181(3) 0.1857(8) 0.0191(14) Uani 1 1 d . . . . .
H5 H 0.298941 0.034538 0.130854 0.023 Uiso 1 1 calc R U . . .
N6 N -0.0886(10) 0.1426(2) 0.2488(6) 0.0206(12) Uani 1 1 d . . . . .
H6A H 0.004324 0.154383 0.324925 0.025 Uiso 1 1 d R U . . .
H6B H -0.232679 0.148955 0.274818 0.025 Uiso 1 1 d R U . . .
C8 C -0.0908(11) 0.2167(2) 0.0727(8) 0.0182(13) Uani 1 1 d . . . . .
H8A H -0.034609 0.228222 -0.036636 0.027 Uiso 1 1 calc R U . . .
H8B H -0.011625 0.235067 0.162756 0.027 Uiso 1 1 calc R U . . .
H8C H -0.261708 0.221751 0.079727 0.027 Uiso 1 1 calc R U . . .
N7B N -0.0376(10) 0.1646(2) 0.0912(7) 0.0215(13) Uani 1 1 d . . . . .
H7BA H -0.119147 0.148151 0.010029 0.026 Uiso 1 1 calc R U . . .
H7BB H 0.118757 0.160274 0.070439 0.026 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 Cl1 2.8860(14) . ?
Pb1 Cl2 2.6755(15) . ?
Pb1 Cl3 3.1971(16) 4_566 ?
Pb1 Cl3 2.8355(15) . ?
Pb1 Cl4 2.9552(14) 1_655 ?
Pb1 Cl4 2.7881(14) . ?
C4 H4 0.9500 . ?
C4 N3 1.328(9) . ?
C4 N1 1.307(9) . ?
N3 H3 0.8800 . ?
N3 C2 1.366(8) . ?
N1 H1 0.8800 . ?
N1 C5 1.371(9) . ?
C2 H2 0.9500 . ?
C2 C5 1.349(10) . ?
C5 H5 0.9500 . ?
N6 H6A 0.8614 . ?
N6 H6B 0.8613 . ?
N6 N7B 1.422(8) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C8 N7B 1.466(8) . ?
N7B H7BA 0.9100 . ?
N7B H7BB 0.9100 . ?

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
Cl1 Pb1 Cl3 93.55(4) . 4_566 ?
Cl1 Pb1 Cl4 83.40(4) . 1_655 ?
Cl2 Pb1 Cl1 90.01(4) . . ?
Cl2 Pb1 Cl3 86.53(5) . . ?
Cl2 Pb1 Cl3 174.21(4) . 4_566 ?
Cl2 Pb1 Cl4 84.11(5) . . ?
Cl2 Pb1 Cl4 82.78(4) . 1_655 ?
Cl3 Pb1 Cl1 173.47(4) . . ?
Cl3 Pb1 Cl3 89.48(2) . 4_566 ?
Cl3 Pb1 Cl4 101.62(4) . 1_655 ?
Cl4 Pb1 Cl1 83.00(4) . . ?
Cl4 Pb1 Cl3 91.79(4) . 4_566 ?
Cl4 Pb1 Cl3 91.13(4) . . ?
Cl4 Pb1 Cl3 102.15(4) 1_655 4_566 ?
Cl4 Pb1 Cl4 161.07(7) . 1_655 ?
Pb1 Cl3 Pb1 143.48(6) . 4_565 ?
Pb1 Cl4 Pb1 161.07(7) . 1_455 ?
N3 C4 H4 125.7 . . ?
N1 C4 H4 125.7 . . ?
N1 C4 N3 108.6(6) . . ?
C4 N3 H3 125.5 . . ?
C4 N3 C2 108.9(6) . . ?
C2 N3 H3 125.5 . . ?
C4 N1 H1 125.5 . . ?
C4 N1 C5 109.0(6) . . ?
C5 N1 H1 125.5 . . ?
N3 C2 H2 126.8 . . ?
C5 C2 N3 106.5(6) . . ?
C5 C2 H2 126.8 . . ?
N1 C5 H5 126.5 . . ?
C2 C5 N1 107.1(6) . . ?
C2 C5 H5 126.5 . . ?
H6A N6 H6B 109.3 . . ?
N7B N6 H6A 109.5 . . ?
N7B N6 H6B 109.0 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N7B C8 H8A 109.5 . . ?
N7B C8 H8B 109.5 . . ?
N7B C8 H8C 109.5 . . ?
N6 N7B C8 117.2(5) . . ?
N6 N7B H7BA 108.0 . . ?
N6 N7B H7BB 108.0 . . ?
C8 N7B H7BA 108.0 . . ?
C8 N7B H7BB 108.0 . . ?
H7BA N7B H7BB 107.2 . . ?

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
C4 H4 Cl2 0.95 2.77 3.499(7) 134.5 1_455 yes
N3 H3 Cl2 0.88 2.57 3.233(5) 132.6 3_556 yes
N3 H3 Cl4 0.88 2.64 3.335(6) 137.0 3_556 yes
N1 H1 N6 0.88 1.98 2.857(8) 173.8 . yes
C2 H2 Cl1 0.95 2.68 3.620(7) 169.1 3_656 yes
C5 H5 Cl1 0.95 2.81 3.642(7) 147.3 1_554 yes
N6 H6A Cl4 0.86 2.82 3.447(5) 131.5 . yes
N7B H7BA Cl1 0.91 2.55 3.252(7) 134.9 1_454 yes
N7B H7BA Cl4 0.91 2.70 3.292(6) 123.3 1_554 yes
N7B H7BB Cl1 0.91 2.34 3.192(6) 156.8 1_554 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
C4 N3 C2 C5 -0.6(7) . . . . ?
C4 N1 C5 C2 -0.8(7) . . . . ?
N3 C4 N1 C5 0.4(7) . . . . ?
N3 C2 C5 N1 0.8(7) . . . . ?
N1 C4 N3 C2 0.1(7) . . . . ?

_olex2_date_sample_data_collection 2022-12-20
_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 3.809
_oxdiff_exptl_absorpt_empirical_full_min 0.665
####################################################################### 
# 
# 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_immhypbbr4_100k
_database_code_depnum_ccdc_archive 'CCDC 2236989'
loop_
_audit_author_name
_audit_author_address
'Dawid Drozdowski'
;Institute of Low Temperature and Structure Research Polish Academy of Sciences
Poland
;
_audit_update_record             
;
2023-01-18 deposited with the CCDC.	2023-03-13 downloaded from the CCDC.
;
_audit_creation_date             2023-01-18
_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, C3 H5 N2, C H7 N2'
_chemical_formula_sum            'C4 H12 Br4 N4 Pb'
_chemical_formula_weight         643.01
_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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   5.9431(2)
_cell_length_b                   28.1818(10)
_cell_length_c                   8.1723(4)
_cell_angle_alpha                90
_cell_angle_beta                 91.129(3)
_cell_angle_gamma                90
_cell_volume                     1368.49(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7637
_cell_measurement_temperature    99.97(13)
_cell_measurement_theta_max      29.1790
_cell_measurement_theta_min      3.2840
_shelx_estimated_absorpt_T_max   0.178
_shelx_estimated_absorpt_T_min   0.044
_exptl_absorpt_coefficient_mu    23.977
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21851
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.121
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.11
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0483
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            13903
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.595
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.97(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6249
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.995
_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    -19.00  91.00   1.00    6.49    --   13.31  57.00  90.00  110
  2  ω    -25.00  30.00   1.00    6.49    --  -14.40 -99.00-150.00   55
  3  ω   -107.00 -35.00   1.00    6.49    --  -14.40-178.00-150.00   72
  4  ω    -23.00  72.00   1.00    6.49    --   13.31  77.00-150.00   95
  5  ω    -65.00  46.00   1.00    6.49    --   13.31 -57.00 120.00  111
;
_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      -0.0450417000
_diffrn_orient_matrix_UB_12      -0.0232575000
_diffrn_orient_matrix_UB_13      -0.0086495000
_diffrn_orient_matrix_UB_21      -0.0110997000
_diffrn_orient_matrix_UB_22      0.0034695000
_diffrn_orient_matrix_UB_23      -0.0859266000
_diffrn_orient_matrix_UB_31      0.1102108000
_diffrn_orient_matrix_UB_32      -0.0091310000
_diffrn_orient_matrix_UB_33      -0.0103743000
_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                2594
_reflns_number_total             2798
_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  (Sheldrick, 2015)'
_refine_diff_density_max         2.360
_refine_diff_density_min         -2.749
_refine_diff_density_rms         0.305
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.167
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     84
_refine_ls_number_reflns         2798
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0394
_refine_ls_restrained_S_all      1.196
_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)+(0.0263P)²+30.5818P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0887
_refine_ls_wR_factor_ref         0.0901
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(Pb1) \\sim Ueq: with sigma of 0.0004 and sigma for terminal atoms of
0.0008
Uanis(N6) = Uanis(N7) = Uanis(C8)
Uanis(N1) = Uanis(C2) = Uanis(C3) = Uanis(N4) = Uanis(C5)
3.a Rotating group:
 N6(H6A,H6B)
3.b Secondary CH2 refined with riding coordinates:
 N7(H7A,H7B)
3.c Aromatic/amide H refined with riding coordinates:
 N4(H4), C3(H3), N1(H1), C2(H2), C5(H5)
3.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C)
;
_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 0.46160(6) 0.17342(2) 0.67874(4) 0.00493(11) Uani 1 1 d . U . . .
Br1 Br 0.46646(16) 0.11660(3) 0.99002(12) 0.0121(2) Uani 1 1 d . . . . .
Br2 Br 0.45897(16) 0.08913(3) 0.48673(12) 0.0113(2) Uani 1 1 d . . . . .
Br3 Br 0.42537(17) 0.22642(4) 0.36429(13) 0.0151(2) Uani 1 1 d . . . . .
Br4 Br -0.03002(15) 0.15993(3) 0.69091(13) 0.0126(2) Uani 1 1 d . . . . .
N4 N -0.0622(15) -0.0373(3) 0.2877(11) 0.0174(9) Uani 1 1 d . . . . .
H4 H -0.120391 -0.064700 0.316600 0.021 Uiso 1 1 calc R U . . .
C3 C 0.1357(19) -0.0310(4) 0.2083(14) 0.0174(9) Uani 1 1 d . . . . .
H3 H 0.234827 -0.055309 0.173473 0.021 Uiso 1 1 calc R U . . .
N1 N -0.0199(15) 0.0376(3) 0.2527(11) 0.0174(9) Uani 1 1 d . . . . .
H1 H -0.044701 0.068378 0.252412 0.021 Uiso 1 1 calc R U . . .
C2 C 0.1639(19) 0.0159(4) 0.1886(14) 0.0174(9) Uani 1 1 d . . . . .
H2 H 0.288201 0.031160 0.139475 0.021 Uiso 1 1 calc R U . . .
C5 C -0.1530(19) 0.0059(4) 0.3143(14) 0.0174(9) Uani 1 1 d . . . . .
H5 H -0.289989 0.012000 0.368379 0.021 Uiso 1 1 calc R U . . .
N6 N -0.0713(17) 0.1401(3) 0.2580(12) 0.0192(13) Uani 1 1 d . . . . .
H6A H 0.012218 0.150162 0.341702 0.023 Uiso 1 1 d R U . . .
H6B H -0.214875 0.145254 0.278255 0.023 Uiso 1 1 d R U . . .
C8 C -0.068(2) 0.2146(4) 0.1000(14) 0.0192(13) Uani 1 1 d . . . . .
H8A H -0.028106 0.226051 -0.009013 0.029 Uiso 1 1 calc R U . . .
H8B H 0.019854 0.232020 0.183266 0.029 Uiso 1 1 calc R U . . .
H8C H -0.228658 0.219815 0.117039 0.029 Uiso 1 1 calc R U . . .
N7 N -0.0177(17) 0.1641(3) 0.1128(12) 0.0192(13) Uani 1 1 d . . . . .
H7A H -0.090877 0.149182 0.028534 0.023 Uiso 1 1 calc R U . . .
H7B H 0.132379 0.160325 0.096890 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 Br1 3.0056(10) . ?
Pb1 Br2 2.8469(10) . ?
Pb1 Br3 3.2135(10) 4_566 ?
Pb1 Br3 2.9764(10) . ?
Pb1 Br4 3.0449(10) 1_655 ?
Pb1 Br4 2.9500(10) . ?
N4 H4 0.8800 . ?
N4 C3 1.366(14) . ?
N4 C5 1.350(14) . ?
C3 H3 0.9500 . ?
C3 C2 1.344(15) . ?
N1 H1 0.8800 . ?
N1 C2 1.365(14) . ?
N1 C5 1.302(14) . ?
C2 H2 0.9500 . ?
C5 H5 0.9500 . ?
N6 H6A 0.8841 . ?
N6 H6B 0.8845 . ?
N6 N7 1.408(13) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C8 N7 1.459(13) . ?
N7 H7A 0.9100 . ?
N7 H7B 0.9100 . ?

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 93.91(3) . 4_566 ?
Br1 Pb1 Br4 85.00(3) . 1_655 ?
Br2 Pb1 Br1 91.25(3) . . ?
Br2 Pb1 Br3 86.75(3) . . ?
Br2 Pb1 Br3 173.40(3) . 4_566 ?
Br2 Pb1 Br4 85.20(3) . . ?
Br2 Pb1 Br4 84.74(3) . 1_655 ?
Br3 Pb1 Br1 175.89(3) . . ?
Br3 Pb1 Br3 87.839(14) . 4_566 ?
Br3 Pb1 Br4 98.38(3) . 1_655 ?
Br4 Pb1 Br1 84.02(3) . . ?
Br4 Pb1 Br3 91.25(3) . 4_566 ?
Br4 Pb1 Br3 92.23(3) . . ?
Br4 Pb1 Br3 99.79(3) 1_655 4_566 ?
Br4 Pb1 Br4 164.92(4) . 1_655 ?
Pb1 Br3 Pb1 147.54(4) . 4_565 ?
Pb1 Br4 Pb1 164.92(4) . 1_455 ?
C3 N4 H4 126.0 . . ?
C5 N4 H4 126.0 . . ?
C5 N4 C3 108.1(9) . . ?
N4 C3 H3 126.4 . . ?
C2 C3 N4 107.1(10) . . ?
C2 C3 H3 126.4 . . ?
C2 N1 H1 125.1 . . ?
C5 N1 H1 125.1 . . ?
C5 N1 C2 109.8(9) . . ?
C3 C2 N1 107.0(10) . . ?
C3 C2 H2 126.5 . . ?
N1 C2 H2 126.5 . . ?
N4 C5 H5 126.0 . . ?
N1 C5 N4 108.0(10) . . ?
N1 C5 H5 126.0 . . ?
H6A N6 H6B 109.3 . . ?
N7 N6 H6A 111.4 . . ?
N7 N6 H6B 108.2 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N7 C8 H8A 109.5 . . ?
N7 C8 H8B 109.5 . . ?
N7 C8 H8C 109.5 . . ?
N6 N7 C8 118.7(8) . . ?
N6 N7 H7A 107.6 . . ?
N6 N7 H7B 107.6 . . ?
C8 N7 H7A 107.6 . . ?
C8 N7 H7B 107.6 . . ?
H7A N7 H7B 107.1 . . ?

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
N4 H4 Br2 0.88 2.69 3.356(9) 133.4 3_556 yes
N4 H4 Br4 0.88 2.83 3.503(9) 134.5 3_556 yes
C3 H3 Br1 0.95 2.83 3.766(11) 168.2 3_656 yes
N1 H1 N6 0.88 2.03 2.904(12) 174.7 . yes
C2 H2 Br1 0.95 2.91 3.746(11) 147.6 1_554 yes
C5 H5 Br2 0.95 2.82 3.597(11) 139.9 1_455 yes
N6 H6A Br4 0.88 2.88 3.585(10) 137.6 . yes
N7 H7A Br1 0.91 2.80 3.475(11) 132.1 1_454 yes
N7 H7A Br4 0.91 2.81 3.449(10) 128.7 1_554 yes
N7 H7B Br1 0.91 2.51 3.345(9) 153.1 1_554 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
N4 C3 C2 N1 -1.5(13) . . . . ?
C3 N4 C5 N1 0.7(12) . . . . ?
C2 N1 C5 N4 -1.7(13) . . . . ?
C5 N4 C3 C2 0.5(13) . . . . ?
C5 N1 C2 C3 2.0(13) . . . . ?

_olex2_date_sample_data_collection 2022-12-20
_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 3.036
_oxdiff_exptl_absorpt_empirical_full_min 0.563
