# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_13pbbr4_0m
_database_code_depnum_ccdc_archive 'CCDC 2174149'
loop_
_audit_author_name
_audit_author_address
'Marta Morana'
;University of Pavia
Italy
;
_audit_update_record             
;
2022-05-22 deposited with the CCDC.	2022-08-02 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT029_13pbbr4_0m          
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.761 Why?
RESPONSE: Crystal quality was low, and we were able to select only one crystal for the data collection. Further measurements on the same crystal did not yield a better completeness.  
;
# end Validation Reply Form

_audit_creation_date             2021-10-07
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br4 Pb, C6 H10 N2'
_chemical_formula_sum            'C6 H10 Br4 N2 Pb'
_chemical_formula_weight         636.99
_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           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   21.784(7)
_cell_length_b                   8.821(3)
_cell_length_c                   7.398(3)
_cell_angle_alpha                90
_cell_angle_beta                 107.214(9)
_cell_angle_gamma                90
_cell_volume                     1357.8(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8793
_cell_measurement_temperature    303.0
_cell_measurement_theta_max      28.85
_cell_measurement_theta_min      2.51
_shelx_estimated_absorpt_T_max   0.378
_shelx_estimated_absorpt_T_min   0.086
_exptl_absorpt_coefficient_mu    24.161
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.4957
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dull dark brown'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    3.116
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_unetI/netI     0.0446
_diffrn_reflns_Laue_measured_fraction_full 0.761
_diffrn_reflns_Laue_measured_fraction_max 0.759
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            1712
_diffrn_reflns_point_group_measured_fraction_full 0.761
_diffrn_reflns_point_group_measured_fraction_max 0.759
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.804
_diffrn_reflns_theta_min         2.508
_diffrn_ambient_temperature      303.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.761
_diffrn_measured_fraction_theta_max 0.759
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1073
_reflns_number_total             1341
_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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.945
_refine_diff_density_min         -1.032
_refine_diff_density_rms         0.181
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     63
_refine_ls_number_reflns         1341
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0352
_refine_ls_restrained_S_all      1.052
_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)+(0.0453P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0835
_refine_ls_wR_factor_ref         0.0902
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C005(H005), C006(H006), C4(H4)
2.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb01 Pb 0.750000 0.750000 0.500000 0.03090(16) Uani 1 2 d S . P . .
Br02 Br 0.61047(4) 0.66824(9) 0.36323(18) 0.0496(3) Uani 1 1 d . . . . .
Br03 Br 0.77138(5) 0.56542(12) 0.18312(19) 0.0543(3) Uani 1 1 d . . . . .
C005 C 0.500000 0.2998(12) 0.250000 0.036(3) Uani 1 2 d S T P . .
H005 H 0.500000 0.405267 0.250000 0.043 Uiso 1 2 calc R U P . .
C006 C 0.500000 -0.0124(11) 0.250000 0.056(5) Uani 1 2 d S T P . .
H006 H 0.500000 -0.117877 0.250000 0.067 Uiso 1 2 calc R U P . .
C2 C 0.4444(4) 0.2192(8) 0.1713(16) 0.035(2) Uani 1 1 d . . . . .
C4 C 0.4440(4) 0.0640(8) 0.1678(17) 0.047(3) Uani 1 1 d . . . . .
H4 H 0.406302 0.011287 0.110473 0.056 Uiso 1 1 calc R U . . .
N1 N 0.3836(3) 0.2976(8) 0.0828(15) 0.052(3) Uani 1 1 d . . . . .
H1A H 0.376686 0.301131 -0.041922 0.062 Uiso 1 1 calc R U . . .
H1B H 0.385634 0.391543 0.128178 0.062 Uiso 1 1 calc R U . . .
H1C H 0.351607 0.247886 0.108242 0.062 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb01 Br02 2.9936(12) 7_666 ?
Pb01 Br02 2.9937(12) . ?
Pb01 Br03 3.0692(13) 6_566 ?
Pb01 Br03 3.0016(14) . ?
Pb01 Br03 3.0692(13) 4_655 ?
Pb01 Br03 3.0015(14) 7_666 ?
C005 H005 0.9300 . ?
C005 C2 1.376(10) 2_655 ?
C005 C2 1.376(10) . ?
C006 H006 0.9300 . ?
C006 C4 1.368(10) 2_655 ?
C006 C4 1.368(10) . ?
C2 C4 1.370(10) . ?
C2 N1 1.465(10) . ?
C4 H4 0.9300 . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br02 Pb01 Br02 180.0 7_666 . ?
Br02 Pb01 Br03 88.97(3) . . ?
Br02 Pb01 Br03 86.39(3) 7_666 4_655 ?
Br02 Pb01 Br03 88.97(3) 7_666 7_666 ?
Br02 Pb01 Br03 86.39(3) . 6_566 ?
Br02 Pb01 Br03 91.03(3) . 7_666 ?
Br02 Pb01 Br03 93.61(3) . 4_655 ?
Br02 Pb01 Br03 91.03(3) 7_666 . ?
Br02 Pb01 Br03 93.61(3) 7_666 6_566 ?
Br03 Pb01 Br03 180.0 6_566 4_655 ?
Br03 Pb01 Br03 79.32(3) . 6_566 ?
Br03 Pb01 Br03 100.68(3) . 4_655 ?
Br03 Pb01 Br03 180.0 7_666 . ?
Br03 Pb01 Br03 79.32(3) 7_666 4_655 ?
Br03 Pb01 Br03 100.68(3) 7_666 6_566 ?
Pb01 Br03 Pb01 142.95(4) . 4_645 ?
C2 C005 H005 121.1 2_655 . ?
C2 C005 H005 121.1 . . ?
C2 C005 C2 117.8(10) . 2_655 ?
C4 C006 H006 119.5 . . ?
C4 C006 H006 119.5 2_655 . ?
C4 C006 C4 121.0(10) 2_655 . ?
C005 C2 N1 120.7(7) . . ?
C4 C2 C005 121.6(8) . . ?
C4 C2 N1 117.7(8) . . ?
C006 C4 C2 119.0(8) . . ?
C006 C4 H4 120.5 . . ?
C2 C4 H4 120.5 . . ?
C2 N1 H1A 109.5 . . ?
C2 N1 H1B 109.5 . . ?
C2 N1 H1C 109.5 . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C005 C2 C4 C006 2.1(16) . . . . ?
C2 C005 C2 C4 -1.1(8) 2_655 . . . ?
C2 C005 C2 N1 -179.2(12) 2_655 . . . ?
C4 C006 C4 C2 -1.0(8) 2_655 . . . ?
N1 C2 C4 C006 -179.8(9) . . . . ?

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

data_13pbbrlong_0ma_a
_database_code_depnum_ccdc_archive 'CCDC 2174150'
loop_
_audit_author_name
_audit_author_address
'Marta Morana'
;University of Pavia
Italy
;
_audit_update_record             
;
2022-05-22 deposited with the CCDC.	2022-08-02 downloaded from the CCDC.
;
_audit_creation_date             2022-01-03
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br6 Pb, 2(C8 H14 N2)'
_chemical_formula_sum            'C16 H28 Br6 N4 Pb'
_chemical_formula_weight         963.07
_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                   10.7571(18)
_cell_length_b                   14.525(3)
_cell_length_c                   8.5545(10)
_cell_angle_alpha                90
_cell_angle_beta                 103.540(4)
_cell_angle_gamma                90
_cell_volume                     1299.4(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    463
_cell_measurement_temperature    299.0
_cell_measurement_theta_max      29.45
_cell_measurement_theta_min      2.81
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    15.727
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.3871
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.461
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1379
_diffrn_reflns_av_unetI/netI     0.1200
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            6279
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        23.130
_diffrn_reflns_theta_max         23.130
_diffrn_reflns_theta_min         2.400
_diffrn_ambient_temperature      299.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1198
_reflns_number_total             1816
_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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.027
_refine_diff_density_min         -1.196
_refine_diff_density_rms         0.260
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     126
_refine_ls_number_reflns         1816
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.1068
_refine_ls_R_factor_gt           0.0560
_refine_ls_restrained_S_all      1.025
_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)+(0.0102P)²+4.5929P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0878
_refine_ls_wR_factor_ref         0.1091
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C00C \\sim C009 \\sim C00A \\sim C008 \\sim C007 \\sim C00E: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
3.a Secondary CH2 refined with riding coordinates:
 C00B(H00H,H00I), C00D(H00J,H00K)
3.b Aromatic/amide H refined with riding coordinates:
 C008(H008), C009(H009), C00A(H00G), C00E(H00L)
3.c Idealised Me refined as rotating group:
 N005(H00A,H00B,H00C), N006(H00D,H00E,H00F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb01 Pb 0.000000 0.500000 0.500000 0.0298(3) Uani 1 2 d S . P . .
Br02 Br 0.05277(19) 0.68916(12) 0.3861(2) 0.0387(5) Uani 1 1 d . . . . .
Br03 Br 0.1157(2) 0.42698(13) 0.2340(2) 0.0425(6) Uani 1 1 d . . . . .
Br04 Br 0.24668(19) 0.47621(13) 0.7576(2) 0.0421(6) Uani 1 1 d . . . . .
N005 N 0.1922(13) 0.6156(9) 1.0435(15) 0.033(4) Uani 1 1 d . . . . .
H00A H 0.203815 0.586873 0.956124 0.040 Uiso 1 1 calc R U . . .
H00B H 0.155345 0.669941 1.015746 0.040 Uiso 1 1 calc R U . . .
H00C H 0.142085 0.581580 1.089898 0.040 Uiso 1 1 calc R U . . .
N006 N 0.8163(14) 0.7215(9) 1.0566(16) 0.038(4) Uani 1 1 d . . . . .
H00D H 0.878431 0.712810 1.005354 0.045 Uiso 1 1 calc R U . . .
H00E H 0.812598 0.673304 1.119716 0.045 Uiso 1 1 calc R U . . .
H00F H 0.832236 0.772211 1.116263 0.045 Uiso 1 1 calc R U . . .
C007 C 0.5784(16) 0.7519(12) 1.0059(18) 0.027(4) Uani 1 1 d . U . . .
C008 C 0.5540(17) 0.8432(12) 1.034(2) 0.038(5) Uani 1 1 d . U . . .
H008 H 0.606511 0.889824 1.011463 0.046 Uiso 1 1 calc R U . . .
C009 C 0.3760(16) 0.7970(12) 1.1373(18) 0.029(4) Uani 1 1 d . U . . .
H009 H 0.308952 0.813186 1.183351 0.035 Uiso 1 1 calc R U . . .
C00A C 0.4500(16) 0.8635(12) 1.097(2) 0.037(5) Uani 1 1 d . U . . .
H00G H 0.430365 0.924807 1.111167 0.044 Uiso 1 1 calc R U . . .
C00B C 0.6907(18) 0.7317(14) 0.936(2) 0.046(6) Uani 1 1 d . . . . .
H00H H 0.698636 0.780881 0.862224 0.055 Uiso 1 1 calc R U . . .
H00I H 0.673575 0.675279 0.873887 0.055 Uiso 1 1 calc R U . . .
C00C C 0.3986(18) 0.7029(14) 1.111(2) 0.039(5) Uani 1 1 d . U . . .
C00D C 0.3210(19) 0.6300(13) 1.161(2) 0.049(6) Uani 1 1 d . . . . .
H00J H 0.306632 0.645581 1.265722 0.059 Uiso 1 1 calc R U . . .
H00K H 0.368576 0.572676 1.172210 0.059 Uiso 1 1 calc R U . . .
C00E C 0.5056(18) 0.6840(13) 1.0481(18) 0.038(5) Uani 1 1 d . U . . .
H00L H 0.527217 0.622934 1.034868 0.046 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb01 Br02 3.0132(19) . ?
Pb01 Br02 3.0133(19) 3_566 ?
Pb01 Br03 3.0298(17) . ?
Pb01 Br03 3.0298(17) 3_566 ?
Pb01 Br04 3.046(2) 3_566 ?
Pb01 Br04 3.046(2) . ?
N005 H00A 0.8900 . ?
N005 H00B 0.8900 . ?
N005 H00C 0.8900 . ?
N005 C00D 1.52(2) . ?
N006 H00D 0.8900 . ?
N006 H00E 0.8900 . ?
N006 H00F 0.8900 . ?
N006 C00B 1.50(2) . ?
C007 C008 1.38(2) . ?
C007 C00B 1.50(2) . ?
C007 C00E 1.36(2) . ?
C008 H008 0.9300 . ?
C008 C00A 1.38(2) . ?
C009 H009 0.9300 . ?
C009 C00A 1.35(2) . ?
C009 C00C 1.41(2) . ?
C00A H00G 0.9300 . ?
C00B H00H 0.9700 . ?
C00B H00I 0.9700 . ?
C00C C00D 1.47(2) . ?
C00C C00E 1.41(2) . ?
C00D H00J 0.9700 . ?
C00D H00K 0.9700 . ?
C00E H00L 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br02 Pb01 Br02 180.0 . 3_566 ?
Br02 Pb01 Br03 86.25(5) 3_566 3_566 ?
Br02 Pb01 Br03 93.75(5) 3_566 . ?
Br02 Pb01 Br03 93.75(5) . 3_566 ?
Br02 Pb01 Br03 86.25(5) . . ?
Br02 Pb01 Br04 98.00(5) 3_566 3_566 ?
Br02 Pb01 Br04 82.00(5) 3_566 . ?
Br02 Pb01 Br04 98.00(5) . . ?
Br02 Pb01 Br04 82.00(5) . 3_566 ?
Br03 Pb01 Br03 180.0 3_566 . ?
Br03 Pb01 Br04 93.56(5) . . ?
Br03 Pb01 Br04 86.44(5) 3_566 . ?
Br03 Pb01 Br04 86.44(5) . 3_566 ?
Br03 Pb01 Br04 93.56(5) 3_566 3_566 ?
Br04 Pb01 Br04 180.0 3_566 . ?
H00A N005 H00B 109.5 . . ?
H00A N005 H00C 109.5 . . ?
H00B N005 H00C 109.5 . . ?
C00D N005 H00A 109.5 . . ?
C00D N005 H00B 109.5 . . ?
C00D N005 H00C 109.5 . . ?
H00D N006 H00E 109.5 . . ?
H00D N006 H00F 109.5 . . ?
H00E N006 H00F 109.5 . . ?
C00B N006 H00D 109.5 . . ?
C00B N006 H00E 109.5 . . ?
C00B N006 H00F 109.5 . . ?
C008 C007 C00B 117.5(16) . . ?
C00E C007 C008 120.4(16) . . ?
C00E C007 C00B 122.1(17) . . ?
C007 C008 H008 120.8 . . ?
C00A C008 C007 118.4(17) . . ?
C00A C008 H008 120.8 . . ?
C00A C009 H009 119.4 . . ?
C00A C009 C00C 121.2(16) . . ?
C00C C009 H009 119.4 . . ?
C008 C00A H00G 119.1 . . ?
C009 C00A C008 121.9(17) . . ?
C009 C00A H00G 119.1 . . ?
N006 C00B H00H 108.5 . . ?
N006 C00B H00I 108.5 . . ?
C007 C00B N006 115.1(13) . . ?
C007 C00B H00H 108.5 . . ?
C007 C00B H00I 108.5 . . ?
H00H C00B H00I 107.5 . . ?
C009 C00C C00D 121.2(17) . . ?
C00E C00C C009 115.8(16) . . ?
C00E C00C C00D 122.7(18) . . ?
N005 C00D H00J 108.9 . . ?
N005 C00D H00K 108.9 . . ?
C00C C00D N005 113.4(14) . . ?
C00C C00D H00J 108.9 . . ?
C00C C00D H00K 108.9 . . ?
H00J C00D H00K 107.7 . . ?
C007 C00E C00C 122.2(17) . . ?
C007 C00E H00L 118.9 . . ?
C00C C00E H00L 118.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C007 C008 C00A C009 3(3) . . . . ?
C008 C007 C00B N006 87(2) . . . . ?
C008 C007 C00E C00C 4(3) . . . . ?
C009 C00C C00D N005 80(2) . . . . ?
C009 C00C C00E C007 -4(3) . . . . ?
C00A C009 C00C C00D 177.6(17) . . . . ?
C00A C009 C00C C00E 3(3) . . . . ?
C00B C007 C008 C00A 179.2(16) . . . . ?
C00B C007 C00E C00C -178.8(16) . . . . ?
C00C C009 C00A C008 -3(3) . . . . ?
C00D C00C C00E C007 -178.4(17) . . . . ?
C00E C007 C008 C00A -4(3) . . . . ?
C00E C007 C00B N006 -90(2) . . . . ?
C00E C00C C00D N005 -105(2) . . . . ?

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

data_14pbbr4_0m_a
_database_code_depnum_ccdc_archive 'CCDC 2174151'
loop_
_audit_author_name
_audit_author_address
'Marta Morana'
;University of Pavia
Italy
;
_audit_update_record             
;
2022-05-22 deposited with the CCDC.	2022-08-02 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_14pbbr4_0m_a        
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.815 Why?  
RESPONSE: Crystal quality was low, and we were able to select only one crystal for the data collection. Further measurements on the same crystal did not yield a better completeness. 
;
# end Validation Reply Form
_audit_creation_date             2021-10-07
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br4 Pb, C6 H10 N2'
_chemical_formula_sum            'C6 H10 Br4 N2 Pb'
_chemical_formula_weight         636.99
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   7.434(3)
_cell_length_b                   8.712(3)
_cell_length_c                   11.028(4)
_cell_angle_alpha                70.570(19)
_cell_angle_beta                 78.527(19)
_cell_angle_gamma                89.414(19)
_cell_volume                     658.9(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2265
_cell_measurement_temperature    302.0
_cell_measurement_theta_max      27.03
_cell_measurement_theta_min      3.63
_shelx_estimated_absorpt_T_max   0.436
_shelx_estimated_absorpt_T_min   0.369
_exptl_absorpt_coefficient_mu    24.894
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5243
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1030 before and 0.0476 after correction.
The Ratio of minimum to maximum transmission is 0.7033.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    3.211
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             564
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0633
_diffrn_reflns_av_unetI/netI     0.1062
_diffrn_reflns_Laue_measured_fraction_full 0.815
_diffrn_reflns_Laue_measured_fraction_max 0.687
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3512
_diffrn_reflns_point_group_measured_fraction_full 0.815
_diffrn_reflns_point_group_measured_fraction_max 0.687
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.196
_diffrn_reflns_theta_min         2.483
_diffrn_ambient_temperature      302.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.815
_diffrn_measured_fraction_theta_max 0.687
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1244
_reflns_number_total             2016
_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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         2.186
_refine_diff_density_min         -2.241
_refine_diff_density_rms         0.371
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     123
_refine_ls_number_reflns         2016
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.1202
_refine_ls_R_factor_gt           0.0653
_refine_ls_restrained_S_all      1.075
_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)+(0.0667P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1346
_refine_ls_wR_factor_ref         0.1710
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H,H) groups
2. Rigid bond restraints
 C009, C00B, C00A, C00C, C00E, C00D
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C00B \\sim C00A \\sim C00C \\sim C00E \\sim C00D \\sim C009: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
4.a Aromatic/amide H refined with riding coordinates:
 C00A(H00G), C00B(H00H), C00D(H00I), C00E(H00J)
4.b Idealised Me refined as rotating group:
 N007(H00A,H00B,H00C), N008(H00D,H00E,H00F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb01 Pb 1.000000 1.000000 0.500000 0.0348(4) Uani 1 2 d S . P . .
Pb02 Pb 0.500000 0.500000 0.500000 0.0341(4) Uani 1 2 d S . P . .
Br03 Br 0.1703(4) 0.6986(3) 0.4560(3) 0.0451(7) Uani 1 1 d . . . . .
Br04 Br 1.0852(4) 1.1549(3) 0.2083(2) 0.0442(7) Uani 1 1 d . . . . .
Br05 Br 0.3653(4) 0.3594(3) 0.7888(2) 0.0453(7) Uani 1 1 d . . . . .
Br06 Br 0.6506(4) 0.8083(4) 0.5249(3) 0.0580(9) Uani 1 1 d . . . . .
N007 N -0.057(3) 0.470(2) 0.7702(18) 0.042(5) Uani 1 1 d . . . . .
H00A H -0.074936 0.446191 0.700795 0.051 Uiso 1 1 calc R U . . .
H00B H 0.061727 0.463052 0.773939 0.051 Uiso 1 1 calc R U . . .
H00C H -0.089793 0.570196 0.763079 0.051 Uiso 1 1 calc R U . . .
N008 N -0.490(3) 0.011(2) 1.2266(19) 0.049(6) Uani 1 1 d . . . . .
H00D H -0.496101 -0.085757 1.216269 0.059 Uiso 1 1 calc R U . . .
H00E H -0.601774 0.047215 1.238424 0.059 Uiso 1 1 calc R U . . .
H00F H -0.441572 0.001027 1.296478 0.059 Uiso 1 1 calc R U . . .
C009 C -0.371(3) 0.128(2) 1.108(2) 0.025(4) Uani 1 1 d . U . . .
C00A C -0.161(4) 0.196(3) 0.904(2) 0.041(6) Uani 1 1 d . U . . .
H00G H -0.087370 0.163463 0.839312 0.049 Uiso 1 1 calc R U . . .
C00B C -0.263(4) 0.081(3) 1.012(2) 0.047(6) Uani 1 1 d . U . . .
H00H H -0.259684 -0.029020 1.019908 0.056 Uiso 1 1 calc R U . . .
C00C C -0.165(3) 0.356(3) 0.888(2) 0.034(5) Uani 1 1 d . U . . .
C00D C -0.377(3) 0.292(3) 1.098(2) 0.042(6) Uani 1 1 d . U . . .
H00I H -0.447554 0.324872 1.162959 0.051 Uiso 1 1 calc R U . . .
C00E C -0.274(3) 0.400(3) 0.988(2) 0.037(5) Uani 1 1 d . U . . .
H00J H -0.275976 0.510334 0.979438 0.045 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb01 Br03 3.045(3) 1_655 ?
Pb01 Br03 3.045(3) 2_676 ?
Pb01 Br04 2.982(3) 2_776 ?
Pb01 Br04 2.982(3) . ?
Pb01 Br06 3.018(3) 2_776 ?
Pb01 Br06 3.018(3) . ?
Pb02 Br03 3.010(3) 2_666 ?
Pb02 Br03 3.010(3) . ?
Pb02 Br05 2.968(3) 2_666 ?
Pb02 Br05 2.968(3) . ?
Pb02 Br06 3.037(3) 2_666 ?
Pb02 Br06 3.037(3) . ?
N007 H00A 0.8900 . ?
N007 H00B 0.8900 . ?
N007 H00C 0.8900 . ?
N007 C00C 1.43(3) . ?
N008 H00D 0.8900 . ?
N008 H00E 0.8900 . ?
N008 H00F 0.8900 . ?
N008 C009 1.48(3) . ?
C009 C00B 1.37(3) . ?
C009 C00D 1.39(3) . ?
C00A H00G 0.9300 . ?
C00A C00B 1.37(3) . ?
C00A C00C 1.34(3) . ?
C00B H00H 0.9300 . ?
C00C C00E 1.40(3) . ?
C00D H00I 0.9300 . ?
C00D C00E 1.35(3) . ?
C00E H00J 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br03 Pb01 Br03 180.0 2_676 1_655 ?
Br04 Pb01 Br03 93.41(7) . 2_676 ?
Br04 Pb01 Br03 93.41(7) 2_776 1_655 ?
Br04 Pb01 Br03 86.59(7) . 1_655 ?
Br04 Pb01 Br03 86.59(7) 2_776 2_676 ?
Br04 Pb01 Br04 180.0 . 2_776 ?
Br04 Pb01 Br06 82.19(8) . 2_776 ?
Br04 Pb01 Br06 97.81(8) . . ?
Br04 Pb01 Br06 82.19(8) 2_776 . ?
Br04 Pb01 Br06 97.81(8) 2_776 2_776 ?
Br06 Pb01 Br03 98.51(8) 2_776 1_655 ?
Br06 Pb01 Br03 98.51(8) . 2_676 ?
Br06 Pb01 Br03 81.49(8) 2_776 2_676 ?
Br06 Pb01 Br03 81.49(8) . 1_655 ?
Br06 Pb01 Br06 180.0 . 2_776 ?
Br03 Pb02 Br03 180.0 . 2_666 ?
Br03 Pb02 Br06 82.42(8) . . ?
Br03 Pb02 Br06 97.58(8) . 2_666 ?
Br03 Pb02 Br06 97.58(8) 2_666 . ?
Br03 Pb02 Br06 82.42(8) 2_666 2_666 ?
Br05 Pb02 Br03 94.00(8) . . ?
Br05 Pb02 Br03 86.00(8) . 2_666 ?
Br05 Pb02 Br03 86.00(8) 2_666 . ?
Br05 Pb02 Br03 94.00(8) 2_666 2_666 ?
Br05 Pb02 Br05 180.00(11) . 2_666 ?
Br05 Pb02 Br06 91.20(8) . . ?
Br05 Pb02 Br06 88.80(8) . 2_666 ?
Br05 Pb02 Br06 88.80(8) 2_666 . ?
Br05 Pb02 Br06 91.20(8) 2_666 2_666 ?
Br06 Pb02 Br06 180.0 2_666 . ?
Pb02 Br03 Pb01 140.42(10) . 1_455 ?
Pb01 Br06 Pb02 143.81(12) . . ?
H00A N007 H00B 109.5 . . ?
H00A N007 H00C 109.5 . . ?
H00B N007 H00C 109.5 . . ?
C00C N007 H00A 109.5 . . ?
C00C N007 H00B 109.5 . . ?
C00C N007 H00C 109.5 . . ?
H00D N008 H00E 109.5 . . ?
H00D N008 H00F 109.5 . . ?
H00E N008 H00F 109.5 . . ?
C009 N008 H00D 109.5 . . ?
C009 N008 H00E 109.5 . . ?
C009 N008 H00F 109.5 . . ?
C00B C009 N008 122.8(19) . . ?
C00B C009 C00D 121(2) . . ?
C00D C009 N008 116(2) . . ?
C00B C00A H00G 119.0 . . ?
C00C C00A H00G 119.0 . . ?
C00C C00A C00B 122(2) . . ?
C009 C00B H00H 120.3 . . ?
C00A C00B C009 119(2) . . ?
C00A C00B H00H 120.3 . . ?
C00A C00C N007 119(2) . . ?
C00A C00C C00E 117(2) . . ?
C00E C00C N007 124(2) . . ?
C009 C00D H00I 121.5 . . ?
C00E C00D C009 117(2) . . ?
C00E C00D H00I 121.5 . . ?
C00C C00E H00J 118.3 . . ?
C00D C00E C00C 123(2) . . ?
C00D C00E H00J 118.3 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N007 C00C C00E C00D 179(2) . . . . ?
N008 C009 C00B C00A 179(2) . . . . ?
N008 C009 C00D C00E -178(2) . . . . ?
C009 C00D C00E C00C 0(4) . . . . ?
C00A C00C C00E C00D -1(4) . . . . ?
C00B C009 C00D C00E 1(4) . . . . ?
C00B C00A C00C N007 -179(2) . . . . ?
C00B C00A C00C C00E 2(4) . . . . ?
C00C C00A C00B C009 -1(4) . . . . ?
C00D C009 C00B C00A -1(4) . . . . ?

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

data_14lonpbbr_0ma_a
_database_code_depnum_ccdc_archive 'CCDC 2174152'
loop_
_audit_author_name
_audit_author_address
'Marta Morana'
;University of Pavia
Italy
;
_audit_update_record             
;
2022-05-22 deposited with the CCDC.	2022-08-02 downloaded from the CCDC.
;
_audit_creation_date             2021-12-28
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br4 Pb, C8 H14 N2'
_chemical_formula_sum            'C8 H14 Br4 N2 Pb'
_chemical_formula_weight         665.04
_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                   12.3274(7)
_cell_length_b                   8.1618(4)
_cell_length_c                   8.1675(4)
_cell_angle_alpha                90
_cell_angle_beta                 90.817(2)
_cell_angle_gamma                90
_cell_volume                     821.68(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7438
_cell_measurement_temperature    299.0
_cell_measurement_theta_max      32.04
_cell_measurement_theta_min      2.99
_shelx_estimated_absorpt_T_max   0.502
_shelx_estimated_absorpt_T_min   0.240
_exptl_absorpt_coefficient_mu    19.969
_exptl_absorpt_correction_T_max  0.7469
_exptl_absorpt_correction_T_min  0.4345
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1002 before and 0.0515 after correction.
The Ratio of minimum to maximum transmission is 0.5817.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.688
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             596
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_unetI/netI     0.0781
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9093
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         35.040
_diffrn_reflns_theta_min         2.993
_diffrn_ambient_temperature      299.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2198
_reflns_number_total             3501
_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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.576
_refine_diff_density_min         -1.861
_refine_diff_density_rms         0.280
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     71
_refine_ls_number_reflns         3501
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0977
_refine_ls_R_factor_gt           0.0526
_refine_ls_restrained_S_all      1.108
_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)+10.2448P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1049
_refine_ls_wR_factor_ref         0.1225
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1D,H1E)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4)
2.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb01 Pb 0.500000 1.000000 0.500000 0.02888(12) Uani 1 2 d S . P . .
N1 N 0.2886(6) 0.5754(10) 0.5727(11) 0.0462(19) Uani 1 1 d . . . . .
H1A H 0.270996 0.677669 0.545463 0.055 Uiso 1 1 calc R U . . .
H1B H 0.359728 0.561273 0.561607 0.055 Uiso 1 1 calc R U . . .
H1C H 0.270681 0.556929 0.676247 0.055 Uiso 1 1 calc R U . . .
C3 C 0.0566(9) 0.3954(18) 0.5982(18) 0.075(4) Uani 1 1 d . . . . .
H3 H 0.093815 0.324965 0.668631 0.089 Uiso 1 1 calc R U . . .
Br02 Br 0.50046(8) 0.81675(11) 0.81624(11) 0.0422(2) Uani 1 1 d . . . . .
C1 C 0.2308(10) 0.4621(16) 0.4667(17) 0.067(3) Uani 1 1 d . . . . .
H1D H 0.252649 0.350927 0.493306 0.080 Uiso 1 1 calc R U . . .
H1E H 0.249968 0.483141 0.353830 0.080 Uiso 1 1 calc R U . . .
Br03 Br 0.25637(8) 0.97823(13) 0.48251(13) 0.0482(2) Uani 1 1 d . . . . .
C2 C 0.1107(7) 0.4778(12) 0.4843(13) 0.046(2) Uani 1 1 d . . . . .
C4 C 0.0543(10) 0.586(2) 0.3877(18) 0.082(5) Uani 1 1 d . . . . .
H4 H 0.091255 0.648719 0.311316 0.099 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb01 Br02 2.9846(8) 3_676 ?
Pb01 Br02 2.9894(8) 4_575 ?
Pb01 Br02 2.9846(8) . ?
Pb01 Br02 2.9894(8) 2_656 ?
Pb01 Br03 3.0099(10) 3_676 ?
Pb01 Br03 3.0099(10) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C1 1.448(14) . ?
C3 H3 0.9300 . ?
C3 C2 1.334(15) . ?
C3 C4 1.381(17) 3_566 ?
C1 H1D 0.9700 . ?
C1 H1E 0.9700 . ?
C1 C2 1.495(15) . ?
C2 C4 1.369(16) . ?
C4 H4 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br02 Pb01 Br02 180.0 3_676 . ?
Br02 Pb01 Br02 89.936(9) . 2_656 ?
Br02 Pb01 Br02 90.064(9) 3_676 2_656 ?
Br02 Pb01 Br02 89.936(9) 3_676 4_575 ?
Br02 Pb01 Br02 90.064(9) . 4_575 ?
Br02 Pb01 Br02 180.0 4_575 2_656 ?
Br02 Pb01 Br03 93.78(3) 2_656 . ?
Br02 Pb01 Br03 90.06(3) . . ?
Br02 Pb01 Br03 89.94(3) 3_676 . ?
Br02 Pb01 Br03 89.94(3) . 3_676 ?
Br02 Pb01 Br03 86.22(3) 4_575 . ?
Br02 Pb01 Br03 93.78(3) 4_575 3_676 ?
Br02 Pb01 Br03 90.06(3) 3_676 3_676 ?
Br02 Pb01 Br03 86.22(3) 2_656 3_676 ?
Br03 Pb01 Br03 180.0 3_676 . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
C2 C3 H3 119.7 . . ?
C2 C3 C4 120.6(11) . 3_566 ?
C4 C3 H3 119.7 3_566 . ?
Pb01 Br02 Pb01 150.21(4) . 2_646 ?
N1 C1 H1D 109.3 . . ?
N1 C1 H1E 109.3 . . ?
N1 C1 C2 111.5(10) . . ?
H1D C1 H1E 108.0 . . ?
C2 C1 H1D 109.3 . . ?
C2 C1 H1E 109.3 . . ?
C3 C2 C1 122.0(10) . . ?
C3 C2 C4 118.2(10) . . ?
C4 C2 C1 119.7(11) . . ?
C3 C4 H4 119.4 3_566 . ?
C2 C4 C3 121.1(12) . 3_566 ?
C2 C4 H4 119.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 -86.9(15) . . . . ?
N1 C1 C2 C4 89.4(15) . . . . ?
C3 C2 C4 C3 -3(3) . . . 3_566 ?
C1 C2 C4 C3 -179.5(13) . . . 3_566 ?
C4 C3 C2 C1 179.4(13) 3_566 . . . ?
C4 C3 C2 C4 3(3) 3_566 . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
