# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_g2_pbca_0p83_a
_database_code_depnum_ccdc_archive 'CCDC 1521054'
_audit_update_record             
;
2016-12-06 deposited with the CCDC.
2017-04-24 downloaded from the CCDC.
;
_audit_creation_date             2016-12-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        'bis(butylammonium) tetrabromoplumbate'
_chemical_formula_moiety         '(Br4 Pb), 2(C4 H12 N)'
_chemical_formula_sum            'C8 H24 Br4 N2 Pb'
_chemical_formula_weight         675.12
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   8.3343(3)
_cell_length_b                   8.2225(4)
_cell_length_c                   27.6171(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1892.57(15)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8085
_cell_measurement_temperature    298
_cell_measurement_theta_max      27.576
_cell_measurement_theta_min      2.855
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    17.341
_exptl_absorpt_correction_T_max  0.3829
_exptl_absorpt_correction_T_min  0.2758
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/2 (Bruker,2014/2) was used for absorption correction.
wR2(int) was 0.1226 before and 0.0559 after correction.
The Ratio of minimum to maximum transmission is 0.7203.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.369
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1232
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.01
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0427
_diffrn_reflns_av_unetI/netI     0.0192
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            28686
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.346
_diffrn_reflns_theta_min         2.855
_diffrn_ambient_temperature      298
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   
;
Advanced Light Source, station 11.3.1
;
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1341
_reflns_number_total             1717
_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       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         0.845
_refine_diff_density_min         -0.624
_refine_diff_density_rms         0.129
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     72
_refine_ls_number_reflns         1717
_refine_ls_number_restraints     26
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0277
_refine_ls_restrained_S_all      1.138
_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)+(0.0299P)²+2.4465P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0605
_refine_ls_wR_factor_ref         0.0660
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C3-C4
 1.54 with sigma of 0.01
 C2-C1 \\sim C3-C2
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C4 \\sim C3 \\sim C2 \\sim C1 \\sim N1: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
4.a Secondary CH2 refined with riding coordinates:
 C1(H1D,H1E), C2(H2A,H2B), C3(H3A,H3B)
4.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), C4(H4A,H4B,H4C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.5000 0.5000 0.5000 0.03541(12) Uani 1 2 d S T P . .
Br2 Br 0.30510(7) 0.19409(7) 0.50256(2) 0.05353(19) Uani 1 1 d . . . . .
Br1 Br 0.46565(8) 0.51992(7) 0.39152(3) 0.05733(19) Uani 1 1 d . . . . .
N1 N 0.0740(6) 0.4274(6) 0.41098(18) 0.0624(14) Uani 1 1 d . U . . .
H1A H 0.0597 0.3239 0.4025 0.075 Uiso 1 1 calc GR . . . .
H1B H 0.0581 0.4382 0.4427 0.075 Uiso 1 1 calc GR . . . .
H1C H 0.1737 0.4577 0.4037 0.075 Uiso 1 1 calc GR . . . .
C1 C -0.0409(10) 0.5305(9) 0.3845(3) 0.084(2) Uani 1 1 d D U . . .
H1D H -0.0277 0.6426 0.3947 0.100 Uiso 1 1 calc R . . . .
H1E H -0.1493 0.4972 0.3925 0.100 Uiso 1 1 calc R . . . .
C2 C -0.0176(9) 0.5196(10) 0.3314(3) 0.096(3) Uani 1 1 d D U . . .
H2A H -0.0331 0.4080 0.3211 0.116 Uiso 1 1 calc R . . . .
H2B H 0.0914 0.5510 0.3234 0.116 Uiso 1 1 calc R . . . .
C3 C -0.1336(11) 0.6282(12) 0.3049(3) 0.123(3) Uani 1 1 d D U . . .
H3A H -0.2425 0.5971 0.3131 0.148 Uiso 1 1 calc R . . . .
H3B H -0.1178 0.7399 0.3153 0.148 Uiso 1 1 calc R . . . .
C4 C -0.1112(13) 0.6173(17) 0.2514(3) 0.178(5) Uani 1 1 d D U . . .
H4A H -0.0016 0.6414 0.2434 0.267 Uiso 1 1 calc GR . . . .
H4B H -0.1806 0.6940 0.2356 0.267 Uiso 1 1 calc GR . . . .
H4C H -0.1369 0.5093 0.2406 0.267 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br2 2.9951(5) . ?
Pb1 Br2 2.9951(5) 5_666 ?
Pb1 Br2 3.0029(5) 8_665 ?
Pb1 Br2 3.0029(5) 4_556 ?
Pb1 Br1 3.0138(7) 5_666 ?
Pb1 Br1 3.0139(7) . ?
Br2 Pb1 3.0029(5) 4_456 ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C1 1.473(9) . ?
C1 H1D 0.9700 . ?
C1 H1E 0.9700 . ?
C1 C2 1.482(11) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C3 1.506(9) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.494(8) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br2 Pb1 Br2 179.999(18) . 5_666 ?
Br2 Pb1 Br2 90.772(6) . 4_556 ?
Br2 Pb1 Br2 89.228(6) 5_666 4_556 ?
Br2 Pb1 Br2 90.772(6) 5_666 8_665 ?
Br2 Pb1 Br2 89.228(6) . 8_665 ?
Br2 Pb1 Br2 180.0 8_665 4_556 ?
Br2 Pb1 Br1 85.068(17) 8_665 . ?
Br2 Pb1 Br1 85.068(17) 4_556 5_666 ?
Br2 Pb1 Br1 91.006(15) . . ?
Br2 Pb1 Br1 94.932(17) 8_665 5_666 ?
Br2 Pb1 Br1 94.932(17) 4_556 . ?
Br2 Pb1 Br1 91.005(15) 5_666 5_666 ?
Br2 Pb1 Br1 88.995(15) 5_666 . ?
Br2 Pb1 Br1 88.994(15) . 5_666 ?
Br1 Pb1 Br1 180.0 5_666 . ?
Pb1 Br2 Pb1 154.82(2) . 4_456 ?
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 . . ?
N1 C1 H1D 109.3 . . ?
N1 C1 H1E 109.3 . . ?
N1 C1 C2 111.7(7) . . ?
H1D C1 H1E 107.9 . . ?
C2 C1 H1D 109.3 . . ?
C2 C1 H1E 109.3 . . ?
C1 C2 H2A 109.4 . . ?
C1 C2 H2B 109.4 . . ?
C1 C2 C3 111.1(7) . . ?
H2A C2 H2B 108.0 . . ?
C3 C2 H2A 109.4 . . ?
C3 C2 H2B 109.4 . . ?
C2 C3 H3A 109.3 . . ?
C2 C3 H3B 109.3 . . ?
H3A C3 H3B 108.0 . . ?
C4 C3 C2 111.4(9) . . ?
C4 C3 H3A 109.3 . . ?
C4 C3 H3B 109.3 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?

_olex2_submission_original_sample_id ERD_50
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_preparation       ', Luminescent'
####################################################################### 
# 
# 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_aj84_twina_a
_database_code_depnum_ccdc_archive 'CCDC 1521053'
_audit_update_record             
;
2016-12-06 deposited with the CCDC.
2017-04-24 downloaded from the CCDC.
;
_audit_creation_date             2015-12-03
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        '1,4-butanediammonium tetrabromoplumbate'
_chemical_formula_moiety         'Br4 Pb, C4 H14 N2'
_chemical_formula_sum            'C4 H14 Br4 N2 Pb'
_chemical_formula_weight         617.00
_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'
N N 0.0061 0.0033 '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'
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                   8.0135(4)
_cell_length_b                   8.4270(4)
_cell_length_c                   10.7367(5)
_cell_angle_alpha                78.957(2)
_cell_angle_beta                 69.565(2)
_cell_angle_gamma                89.5420(10)
_cell_volume                     665.47(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9890
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      27.790
_cell_measurement_theta_min      3.547
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    24.642
_exptl_absorpt_correction_T_max  0.431131
_exptl_absorpt_correction_T_min  0.199471
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0675 before and 0.0419 after correction.
 The Ratio of minimum to maximum transmission is 0.47.
 The λ/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.1445 before and 0.0562 after correction.
 The Ratio of minimum to maximum transmission is 0.47.
 The λ/2 correction factor is Not present

Final HKLF 4 output contains 41772 reflections, Rint = 0.0452
 (24730 with I > 3sig(I), Rint = 0.0373)
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.079
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             548
_exptl_crystal_preparation       ', Luminescent'
_exptl_crystal_recrystallization_method 'vapor diffusion into HBr'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0432
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6236
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.277
_diffrn_reflns_theta_min         2.468
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4683
_reflns_number_total             6236
_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         1.304
_refine_diff_density_min         -1.236
_refine_diff_density_rms         0.189
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     106
_refine_ls_number_reflns         6236
_refine_ls_number_restraints     40
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0378
_refine_ls_restrained_S_all      1.035
_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)+(0.0316P)²+3.0203P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0712
_refine_ls_wR_factor_ref         0.0790
_refine_special_details          'Refined as a 2-component twin., Twin'
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.841(3) 0.159(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H) groups
3. Restrained distances
 C2-C3
 1.54 with sigma of 0.02
4. Rigid bond restraints
 N1, C1, C2, C3, C4, N2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
N1 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim N2: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08
6.a Secondary CH2 refined with riding coordinates:
 C1(H1D,H1E), C4(H4A,H4B), C2(H2D,H2E), C3(H3A,H3B)
6.b Idealised Me refined as rotating group:
 N2(H2A,H2B,H2C), 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
Pb1 Pb 0.5000 0.0000 0.5000 0.03073(12) Uani 1 2 d S T P . .
Pb2 Pb 0.0000 0.5000 0.5000 0.03089(12) Uani 1 2 d S T P . .
Br4 Br 0.32890(12) 0.71155(12) 0.44981(10) 0.0474(2) Uani 1 1 d . . . . .
Br2 Br 0.21865(12) 0.21190(12) 0.44638(10) 0.0483(2) Uani 1 1 d . . . . .
Br1 Br 0.70893(13) 0.10775(13) 0.20558(10) 0.0506(2) Uani 1 1 d . . . . .
Br3 Br -0.06859(13) 0.38899(12) 0.79598(10) 0.0488(2) Uani 1 1 d . . . . .
N2 N 1.3498(11) 0.4974(11) -0.2420(9) 0.059(2) Uani 1 1 d . U . . .
H2A H 1.4216 0.4541 -0.3092 0.071 Uiso 1 1 calc GR . . . .
H2B H 1.3547 0.6044 -0.2693 0.071 Uiso 1 1 calc GR . . . .
H2C H 1.2384 0.4571 -0.2188 0.071 Uiso 1 1 calc GR . . . .
N1 N 1.0927(11) -0.0011(10) 0.2450(9) 0.054(2) Uani 1 1 d . U . . .
H1A H 0.9931 0.0220 0.2283 0.065 Uiso 1 1 calc GR . . . .
H1B H 1.1000 0.0516 0.3075 0.065 Uiso 1 1 calc GR . . . .
H1C H 1.0912 -0.1073 0.2754 0.065 Uiso 1 1 calc GR . . . .
C1 C 1.2477(14) 0.0489(12) 0.1197(11) 0.057(3) Uani 1 1 d . U . . .
H1D H 1.2493 -0.0197 0.0563 0.069 Uiso 1 1 calc R . . . .
H1E H 1.3565 0.0358 0.1399 0.069 Uiso 1 1 calc R . . . .
C4 C 1.4069(17) 0.4589(12) -0.1251(11) 0.061(3) Uani 1 1 d . U . . .
H4A H 1.3341 0.5143 -0.0555 0.073 Uiso 1 1 calc R . . . .
H4B H 1.5295 0.5008 -0.1524 0.073 Uiso 1 1 calc R . . . .
C2 C 1.2402(15) 0.2246(12) 0.0556(12) 0.067(3) Uani 1 1 d D U . . .
H2D H 1.1337 0.2357 0.0321 0.080 Uiso 1 1 calc R . . . .
H2E H 1.2311 0.2915 0.1216 0.080 Uiso 1 1 calc R . . . .
C3 C 1.395(2) 0.2833(13) -0.0652(11) 0.084(4) Uani 1 1 d D U . . .
H3A H 1.3959 0.2229 -0.1338 0.101 Uiso 1 1 calc R . . . .
H3B H 1.5013 0.2593 -0.0433 0.101 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br4 3.0249(9) 2_666 ?
Pb1 Br4 3.0249(9) 1_545 ?
Pb1 Br2 3.0085(8) 2_656 ?
Pb1 Br2 3.0085(8) . ?
Pb1 Br1 2.9747(10) 2_656 ?
Pb1 Br1 2.9748(10) . ?
Pb2 Br4 3.0216(8) . ?
Pb2 Br4 3.0217(8) 2_566 ?
Pb2 Br2 3.0098(8) 2_566 ?
Pb2 Br2 3.0098(8) . ?
Pb2 Br3 2.9876(10) 2_566 ?
Pb2 Br3 2.9876(10) . ?
Br4 Pb1 3.0249(9) 1_565 ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 H2C 0.8900 . ?
N2 C4 1.461(13) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C1 1.468(12) . ?
C1 H1D 0.9700 . ?
C1 H1E 0.9700 . ?
C1 C2 1.519(14) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C3 1.485(14) . ?
C2 H2D 0.9700 . ?
C2 H2E 0.9700 . ?
C2 C3 1.452(13) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br4 Pb1 Br4 180.0 2_666 1_545 ?
Br2 Pb1 Br4 90.83(3) 2_656 2_666 ?
Br2 Pb1 Br4 89.17(3) . 2_666 ?
Br2 Pb1 Br4 89.17(3) 2_656 1_545 ?
Br2 Pb1 Br4 90.83(3) . 1_545 ?
Br2 Pb1 Br2 180.0 2_656 . ?
Br1 Pb1 Br4 91.69(3) . 1_545 ?
Br1 Pb1 Br4 91.69(3) 2_656 2_666 ?
Br1 Pb1 Br4 88.31(3) . 2_666 ?
Br1 Pb1 Br4 88.31(3) 2_656 1_545 ?
Br1 Pb1 Br2 94.13(3) . 2_656 ?
Br1 Pb1 Br2 85.87(3) . . ?
Br1 Pb1 Br2 94.13(3) 2_656 . ?
Br1 Pb1 Br2 85.87(3) 2_656 2_656 ?
Br1 Pb1 Br1 180.0 2_656 . ?
Br4 Pb2 Br4 180.0 . 2_566 ?
Br2 Pb2 Br4 91.46(3) 2_566 2_566 ?
Br2 Pb2 Br4 91.46(3) . . ?
Br2 Pb2 Br4 88.54(3) 2_566 . ?
Br2 Pb2 Br4 88.54(3) . 2_566 ?
Br2 Pb2 Br2 180.0 . 2_566 ?
Br3 Pb2 Br4 94.11(3) 2_566 2_566 ?
Br3 Pb2 Br4 85.89(3) 2_566 . ?
Br3 Pb2 Br4 85.89(3) . 2_566 ?
Br3 Pb2 Br4 94.11(3) . . ?
Br3 Pb2 Br2 89.01(3) 2_566 2_566 ?
Br3 Pb2 Br2 90.99(3) 2_566 . ?
Br3 Pb2 Br2 90.99(3) . 2_566 ?
Br3 Pb2 Br2 89.01(3) . . ?
Br3 Pb2 Br3 180.0 . 2_566 ?
Pb2 Br4 Pb1 149.79(4) . 1_565 ?
Pb1 Br2 Pb2 148.42(4) . . ?
H2A N2 H2B 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
C4 N2 H2A 109.5 . . ?
C4 N2 H2B 109.5 . . ?
C4 N2 H2C 109.5 . . ?
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 . . ?
N1 C1 H1D 109.5 . . ?
N1 C1 H1E 109.5 . . ?
N1 C1 C2 110.6(8) . . ?
H1D C1 H1E 108.1 . . ?
C2 C1 H1D 109.5 . . ?
C2 C1 H1E 109.5 . . ?
N2 C4 H4A 108.6 . . ?
N2 C4 H4B 108.6 . . ?
N2 C4 C3 114.6(10) . . ?
H4A C4 H4B 107.6 . . ?
C3 C4 H4A 108.6 . . ?
C3 C4 H4B 108.6 . . ?
C1 C2 H2D 109.0 . . ?
C1 C2 H2E 109.0 . . ?
H2D C2 H2E 107.8 . . ?
C3 C2 C1 113.0(9) . . ?
C3 C2 H2D 109.0 . . ?
C3 C2 H2E 109.0 . . ?
C4 C3 H3A 108.3 . . ?
C4 C3 H3B 108.3 . . ?
C2 C3 C4 116.1(10) . . ?
C2 C3 H3A 108.3 . . ?
C2 C3 H3B 108.3 . . ?
H3A C3 H3B 107.4 . . ?

_olex2_submission_original_sample_id AJ84
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.841(3)
2 0.159(3)

####################################################################### 
# 
# 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_g1_mono_p_0p70_a
_database_code_depnum_ccdc_archive 'CCDC 1521058'
_audit_update_record             
;
2016-12-06 deposited with the CCDC.
2017-04-24 downloaded from the CCDC.
;
_audit_creation_date             2015-11-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        'histammonium tetrabromoplumbate'
_chemical_formula_moiety         'Br4 Pb, C5 H11 N3'
_chemical_formula_sum            'C5 H11 Br4 N3 Pb'
_chemical_formula_weight         640.00
_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'
N N 0.0061 0.0033 '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'
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                   10.6055(13)
_cell_length_b                   11.6091(14)
_cell_length_c                   11.9312(14)
_cell_angle_alpha                90
_cell_angle_beta                 110.061(3)
_cell_angle_gamma                90
_cell_volume                     1379.8(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9997
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      32.760
_cell_measurement_theta_min      2.526
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    23.777
_exptl_absorpt_correction_T_max  0.3404
_exptl_absorpt_correction_T_min  0.1374
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/2 (Bruker,2014/2) was used for absorption correction.
wR2(int) was 0.1360 before and 0.0569 after correction.
The Ratio of minimum to maximum transmission is 0.4036.
The λ/2 correction factor is Not present.
;
_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    3.081
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1136
_exptl_crystal_preparation       ', Luminescent'
_exptl_crystal_recrystallization_method 'Slowly cooled from conc. HBr'
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            31826
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.510
_diffrn_reflns_theta_min         2.526
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3697
_reflns_number_total             4219
_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       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         1.390
_refine_diff_density_min         -1.561
_refine_diff_density_rms         0.193
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     119
_refine_ls_number_reflns         4219
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.0230
_refine_ls_restrained_S_all      1.065
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0307P)²+0.5211P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0540
_refine_ls_wR_factor_ref         0.0562
_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) groups, All N(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C1(H1D,H1E)
2.b Aromatic/amide H refined with riding coordinates:
 N2(H2), N3(H3), C5(H5), 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
Pb1 Pb 0.48687(2) 0.77180(2) 0.75928(2) 0.02612(5) Uani 1 1 d . . . . .
Br1 Br 0.77876(4) 0.72793(3) 0.86665(3) 0.04125(9) Uani 1 1 d . . . . .
Br4 Br 0.44109(5) 0.52225(3) 0.76012(3) 0.04529(10) Uani 1 1 d . . . . .
Br2 Br 0.19031(4) 0.80821(3) 0.63775(4) 0.04574(9) Uani 1 1 d . . . . .
Br3 Br 0.49835(5) 0.74472(4) 0.51908(3) 0.04866(11) Uani 1 1 d . . . . .
N1 N 1.2711(4) 0.4939(3) 0.9658(3) 0.0441(7) Uani 1 1 d . . . . .
H1A H 1.3282 0.5260 0.9350 0.053 Uiso 1 1 calc GR . . . .
H1B H 1.3099 0.4333 1.0098 0.053 Uiso 1 1 calc GR . . . .
H1C H 1.2487 0.5451 1.0112 0.053 Uiso 1 1 calc GR . . . .
N2 N 0.8331(3) 0.5583(3) 0.6639(3) 0.0467(8) Uani 1 1 d . . . . .
H2 H 0.8112 0.6131 0.7021 0.056 Uiso 1 1 calc R . . . .
N3 N 0.8181(4) 0.4282(3) 0.5366(3) 0.0581(10) Uani 1 1 d . . . . .
H3 H 0.7857 0.3826 0.4768 0.070 Uiso 1 1 calc R . . . .
C5 C 0.7504(5) 0.5056(4) 0.5701(4) 0.0585(12) Uani 1 1 d . . . . .
H5 H 0.6593 0.5211 0.5341 0.070 Uiso 1 1 calc R . . . .
C3 C 0.9591(4) 0.5131(3) 0.6920(3) 0.0397(8) Uani 1 1 d . . . . .
C4 C 0.9479(4) 0.4303(4) 0.6102(4) 0.0519(10) Uani 1 1 d . . . . .
H4 H 1.0166 0.3832 0.6051 0.062 Uiso 1 1 calc R . . . .
C2 C 1.0743(5) 0.5540(4) 0.7958(4) 0.0546(11) Uani 1 1 d . . . . .
H2A H 1.1343 0.5990 0.7675 0.065 Uiso 1 1 calc R . . . .
H2B H 1.0414 0.6035 0.8453 0.065 Uiso 1 1 calc R . . . .
C1 C 1.1489(4) 0.4561(3) 0.8679(3) 0.0463(9) Uani 1 1 d . . . . .
H1D H 1.1743 0.4032 0.8165 0.056 Uiso 1 1 calc R . . . .
H1E H 1.0906 0.4152 0.9017 0.056 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br1 2.9602(5) . ?
Pb1 Br4 2.9380(5) . ?
Pb1 Br4 3.0351(5) 2_656 ?
Pb1 Br2 3.0074(5) . ?
Pb1 Br3 3.0660(5) 4_576 ?
Pb1 Br3 2.9269(5) . ?
Br4 Pb1 3.0352(5) 2_646 ?
Br3 Pb1 3.0660(5) 4_575 ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C1 1.482(5) . ?
N2 H2 0.8600 . ?
N2 C5 1.313(5) . ?
N2 C3 1.365(5) . ?
N3 H3 0.8600 . ?
N3 C5 1.296(6) . ?
N3 C4 1.355(5) . ?
C5 H5 0.9300 . ?
C3 C4 1.346(5) . ?
C3 C2 1.488(6) . ?
C4 H4 0.9300 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C1 1.480(5) . ?
C1 H1D 0.9700 . ?
C1 H1E 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br1 Pb1 Br4 86.823(12) . 2_656 ?
Br1 Pb1 Br2 176.645(11) . . ?
Br1 Pb1 Br3 83.035(13) . 4_576 ?
Br4 Pb1 Br1 88.761(12) . . ?
Br4 Pb1 Br4 172.328(6) . 2_656 ?
Br4 Pb1 Br2 89.630(13) . . ?
Br4 Pb1 Br3 102.313(11) 2_656 4_576 ?
Br4 Pb1 Br3 83.351(11) . 4_576 ?
Br2 Pb1 Br4 94.448(13) . 2_656 ?
Br2 Pb1 Br3 99.703(13) . 4_576 ?
Br3 Pb1 Br1 90.955(13) . . ?
Br3 Pb1 Br4 86.106(12) . 2_656 ?
Br3 Pb1 Br4 87.699(12) . . ?
Br3 Pb1 Br2 86.038(14) . . ?
Br3 Pb1 Br3 169.307(9) . 4_576 ?
Pb1 Br4 Pb1 153.911(18) . 2_646 ?
Pb1 Br3 Pb1 174.915(18) . 4_575 ?
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 . . ?
C5 N2 H2 125.0 . . ?
C5 N2 C3 110.0(3) . . ?
C3 N2 H2 125.0 . . ?
C5 N3 H3 125.2 . . ?
C5 N3 C4 109.6(4) . . ?
C4 N3 H3 125.2 . . ?
N2 C5 H5 126.1 . . ?
N3 C5 N2 107.8(4) . . ?
N3 C5 H5 126.1 . . ?
N2 C3 C2 122.5(4) . . ?
C4 C3 N2 105.1(3) . . ?
C4 C3 C2 132.4(4) . . ?
N3 C4 H4 126.3 . . ?
C3 C4 N3 107.4(4) . . ?
C3 C4 H4 126.3 . . ?
C3 C2 H2A 109.4 . . ?
C3 C2 H2B 109.4 . . ?
H2A C2 H2B 108.0 . . ?
C1 C2 C3 111.2(4) . . ?
C1 C2 H2A 109.4 . . ?
C1 C2 H2B 109.4 . . ?
N1 C1 H1D 109.1 . . ?
N1 C1 H1E 109.1 . . ?
C2 C1 N1 112.3(3) . . ?
C2 C1 H1D 109.1 . . ?
C2 C1 H1E 109.1 . . ?
H1D C1 H1E 107.9 . . ?

_olex2_exptl_crystal_mounting_method 
'Mounted on a Mitegen loop using a trace of paratone'
_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_aj97b_a
_database_code_depnum_ccdc_archive 'CCDC 1521067'
_audit_update_record             
;
2016-12-06 deposited with the CCDC.
2017-04-24 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT041_aj97b_a             
;
PROBLEM: Calc. and Reported SumFormula    Strings  Differ     Please Check
RESPONSE: Due to disorder, one H atom cannot be placed, but it was added into the formula
;
_vrf_PLAT043_aj97b_a             
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..       1.02 Check
RESPONSE: Due to disorder, one H atom cannot be placed, but it was added into the formula
;
# Added during the CSD deposition process: Tuesday 06 December 2016 09:24 PM
# end Validation Reply Form

_audit_creation_date             2016-09-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        
'(2-methyl-1,5-pentanediammonium) tetrabromoplumbate'
_chemical_formula_moiety         '0.5(Br8 Pb2), 0.5(C12 H36 N4)'
_chemical_formula_sum            'C6 H18 Br4 N2 Pb'
_chemical_formula_weight         645.04
_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           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                   24.4632(15)
_cell_length_b                   8.0039(4)
_cell_length_c                   8.1963(5)
_cell_angle_alpha                90
_cell_angle_beta                 99.745(2)
_cell_angle_gamma                90
_cell_volume                     1581.69(16)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    298
_cell_measurement_theta_max      26.422
_cell_measurement_theta_min      2.682
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    20.742
_exptl_absorpt_correction_T_max  0.4296
_exptl_absorpt_correction_T_min  0.2402
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/2 (Bruker,2014/2) was used for absorption correction.
wR2(int) was 0.1041 before and 0.0506 after correction.
The Ratio of minimum to maximum transmission is 0.5591.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.705
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1156
_exptl_crystal_preparation       
'Diethyl ether vapor diffusion into concentrated HBr, Luminescent'
_exptl_crystal_recrystallization_method 
'Diethyl ether vapor diffusion into concentrated HBr'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_unetI/netI     0.0103
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            33452
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.017
_diffrn_reflns_theta_min         2.681
_diffrn_ambient_temperature      298
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1404
_reflns_number_total             1548
_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       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         0.969
_refine_diff_density_min         -0.724
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     87
_refine_ls_number_reflns         1548
_refine_ls_number_restraints     77
_refine_ls_R_factor_all          0.0239
_refine_ls_R_factor_gt           0.0199
_refine_ls_restrained_S_all      1.073
_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)+(0.0187P)²+7.2882P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0430
_refine_ls_wR_factor_ref         0.0446
_refine_special_details          
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C-N1 ∼ N1-C0AA
 with sigma of 0.02
 C-C2 ∼ C2-C0AA
 with sigma of 0.02
 C4A-C2 ∼ C2-C4
 with sigma of 0.02
3. Rigid bond restraints
 C3, C2, C4, C4A, C, C0AA, N1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
N1 ∼ C ∼ C0AA ∼ C4 ∼ C4A ∼ C2 ∼ C3: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
5. Others
 Sof(H1BD)=Sof(H1BE)=Sof(H1BF)=Sof(H2B)=Sof(C)=Sof(HA)=Sof(HB)=1-FVAR(1)
 Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(H4AC)=0.5*(1-FVAR(2))
 Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=0.5*FVAR(2)
 Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(H2A)=Sof(C0AA)=Sof(H0AA)=Sof(H0AB)=FVAR(1)
 Fixed Sof: H3A(0.5) H3B(0.5)
6.a Ternary CH refined with riding coordinates:
 C2(H2A), C2(H2B)
6.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C0AA(H0AA,H0AB), C(HA,HB)
6.c Me refined with riding coordinates:
 N1(H1AA,H1AB,H1AC), N1(H1BD,H1BE,H1BF)
6.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C4A(H4AA,H4AB,H4AC)
Due to positional disorder of the organic molecule, methyl group at the
2-position is present with 0.5 occupancy. The other half of the time,
that position is occupied by a hydrogen. This hydrogen was not refined
but the formula was adjusted to include it.
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.2500 0.7500 0.5000 0.03564(8) Uani 1 2 d S T P . .
Br1 Br 0.26870(2) 0.43711(7) 0.69914(6) 0.05922(15) Uani 1 1 d . . . . .
Br2 Br 0.37188(2) 0.81153(8) 0.58637(7) 0.06373(15) Uani 1 1 d . . . . .
N1 N 0.35902(18) 0.2275(6) 0.4965(6) 0.0673(13) Uani 1 1 d D U . . .
H1AA H 0.3278 0.2870 0.4818 0.081 Uiso 0.61(2) 1 calc R . . A 1
H1AB H 0.3710 0.2174 0.4004 0.081 Uiso 0.61(2) 1 calc R . . A 1
H1AC H 0.3525 0.1266 0.5346 0.081 Uiso 0.61(2) 1 calc R . . A 1
H1BD H 0.3372 0.2789 0.4137 0.081 Uiso 0.39(2) 1 calc R . . A 2
H1BE H 0.3627 0.1206 0.4705 0.081 Uiso 0.39(2) 1 calc R . . A 2
H1BF H 0.3440 0.2344 0.5879 0.081 Uiso 0.39(2) 1 calc R . . A 2
C2 C 0.4537(3) 0.2377(8) 0.6559(10) 0.088(2) Uani 1 1 d D U . . .
H2A H 0.4506 0.1227 0.6944 0.106 Uiso 0.61(2) 1 calc R . . A 1
H2B H 0.4363 0.1590 0.7232 0.106 Uiso 0.39(2) 1 calc R . . A 2
C3 C 0.5000 0.3215(13) 0.7500 0.101(3) Uani 1 2 d S TU P A .
H3A H 0.4852 0.3941 0.8266 0.122 Uiso 0.5 1 calc R . . . .
H3B H 0.5148 0.3941 0.6734 0.122 Uiso 0.5 1 calc R . . . .
C0AA C 0.4019(4) 0.3138(15) 0.618(2) 0.069(4) Uani 0.61(2) 1 d D U . A 1
H0AA H 0.4072 0.4248 0.5758 0.083 Uiso 0.61(2) 1 calc R . . A 1
H0AB H 0.3873 0.3273 0.7201 0.083 Uiso 0.61(2) 1 calc R . . A 1
C4 C 0.4796(11) 0.244(4) 0.481(4) 0.108(9) Uani 0.304(11) 1 d D U . A 1
H4A H 0.5138 0.1819 0.4954 0.162 Uiso 0.304(11) 1 calc GR . . A 1
H4B H 0.4865 0.3576 0.4544 0.162 Uiso 0.304(11) 1 calc GR . . A 1
H4C H 0.4536 0.1948 0.3934 0.162 Uiso 0.304(11) 1 calc GR . . A 1
C C 0.4145(6) 0.309(2) 0.525(3) 0.066(5) Uani 0.39(2) 1 d D U . A 2
HA H 0.4298 0.3035 0.4238 0.079 Uiso 0.39(2) 1 calc R . . A 2
HB H 0.4097 0.4260 0.5502 0.079 Uiso 0.39(2) 1 calc R . . A 2
C4A C 0.481(2) 0.142(7) 0.509(6) 0.127(17) Uani 0.196(11) 1 d D U . A 2
H4AA H 0.4900 0.0294 0.5423 0.191 Uiso 0.196(11) 1 calc GR . . A 2
H4AB H 0.5138 0.2003 0.4925 0.191 Uiso 0.196(11) 1 calc GR . . A 2
H4AC H 0.4544 0.1425 0.4083 0.191 Uiso 0.196(11) 1 calc GR . . A 2


_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 2.9820(5) 7_566 ?
Pb1 Br1 2.9820(5) . ?
Pb1 Br1 2.9858(5) 6_565 ?
Pb1 Br1 2.9858(5) 4_556 ?
Pb1 Br2 2.9863(5) 7_566 ?
Pb1 Br2 2.9864(5) . ?
Br1 Pb1 2.9858(5) 4_546 ?
N1 H1AA 0.8900 . ?
N1 H1AB 0.8900 . ?
N1 H1AC 0.8900 . ?
N1 H1BD 0.8900 . ?
N1 H1BE 0.8900 . ?
N1 H1BF 0.8900 . ?
N1 C0AA 1.488(10) . ?
N1 C 1.488(13) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 C3 1.426(8) . ?
C2 C0AA 1.392(10) . ?
C2 C4 1.66(3) . ?
C2 C 1.429(13) . ?
C2 C4A 1.65(3) . ?
C3 C2 1.426(8) 2_656 ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C0AA H0AA 0.9700 . ?
C0AA H0AB 0.9700 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C HA 0.9700 . ?
C HB 0.9700 . ?
C4A H4AA 0.9600 . ?
C4A H4AB 0.9600 . ?
C4A H4AC 0.9600 . ?

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 180.0 7_566 . ?
Br1 Pb1 Br1 90.003(7) . 6_565 ?
Br1 Pb1 Br1 89.996(7) 7_566 6_565 ?
Br1 Pb1 Br1 89.997(7) . 4_556 ?
Br1 Pb1 Br1 90.004(7) 7_566 4_556 ?
Br1 Pb1 Br1 180.000(10) 6_565 4_556 ?
Br1 Pb1 Br2 92.624(17) 7_566 . ?
Br1 Pb1 Br2 90.452(16) 6_565 7_566 ?
Br1 Pb1 Br2 89.548(16) 6_565 . ?
Br1 Pb1 Br2 89.548(16) 4_556 7_566 ?
Br1 Pb1 Br2 87.375(16) 7_566 7_566 ?
Br1 Pb1 Br2 92.626(16) . 7_566 ?
Br1 Pb1 Br2 90.452(16) 4_556 . ?
Br1 Pb1 Br2 87.374(17) . . ?
Br2 Pb1 Br2 180.0 7_566 . ?
Pb1 Br1 Pb1 147.41(2) . 4_546 ?
H1AA N1 H1AB 109.5 . . ?
H1AA N1 H1AC 109.5 . . ?
H1AB N1 H1AC 109.5 . . ?
H1BD N1 H1BE 109.5 . . ?
H1BD N1 H1BF 109.5 . . ?
H1BE N1 H1BF 109.5 . . ?
C0AA N1 H1AA 109.5 . . ?
C0AA N1 H1AB 109.5 . . ?
C0AA N1 H1AC 109.5 . . ?
C N1 H1BD 109.5 . . ?
C N1 H1BE 109.5 . . ?
C N1 H1BF 109.5 . . ?
C3 C2 H2A 111.5 . . ?
C3 C2 H2B 112.2 . . ?
C3 C2 C4 93.9(13) . . ?
C3 C2 C 126.0(9) . . ?
C3 C2 C4A 103(2) . . ?
C0AA C2 H2A 111.5 . . ?
C0AA C2 C3 121.6(8) . . ?
C0AA C2 C4 105.1(12) . . ?
C4 C2 H2A 111.5 . . ?
C C2 H2B 112.2 . . ?
C C2 C4A 87(2) . . ?
C4A C2 H2B 112.2 . . ?
C2 C3 C2 123.8(9) . 2_656 ?
C2 C3 H3A 106.4 2_656 . ?
C2 C3 H3A 106.4 . . ?
C2 C3 H3B 106.4 . . ?
C2 C3 H3B 106.4 2_656 . ?
H3A C3 H3B 106.4 . . ?
N1 C0AA H0AA 108.0 . . ?
N1 C0AA H0AB 108.0 . . ?
C2 C0AA N1 117.2(8) . . ?
C2 C0AA H0AA 108.0 . . ?
C2 C0AA H0AB 108.0 . . ?
H0AA C0AA H0AB 107.2 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N1 C HA 108.5 . . ?
N1 C HB 108.5 . . ?
C2 C N1 115.0(10) . . ?
C2 C HA 108.5 . . ?
C2 C HB 108.5 . . ?
HA C HB 107.5 . . ?
C2 C4A H4AA 109.5 . . ?
C2 C4A H4AB 109.5 . . ?
C2 C4A H4AC 109.5 . . ?
H4AA C4A H4AB 109.5 . . ?
H4AA C4A H4AC 109.5 . . ?
H4AB C4A H4AC 109.5 . . ?

####################################################################### 
# 
# 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_g1_mono_p_0p65_a
_database_code_depnum_ccdc_archive 'CCDC 1521057'
_audit_update_record             
;
2016-12-06 deposited with the CCDC.
2017-04-24 downloaded from the CCDC.
;
_audit_creation_date             2015-12-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        'histammonium tetrabromoplumbate'
_chemical_formula_moiety         'Br4 Pb, C5 H11 N3'
_chemical_formula_sum            'C5 H11 Br4 N3 Pb'
_chemical_formula_weight         640.00
_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                   10.5412(13)
_cell_length_b                   11.5023(14)
_cell_length_c                   11.9250(14)
_cell_angle_alpha                90
_cell_angle_beta                 109.996(3)
_cell_angle_gamma                90
_cell_volume                     1358.7(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9286
_cell_measurement_temperature    100
_cell_measurement_theta_max      35.091
_cell_measurement_theta_min      2.538
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    24.147
_exptl_absorpt_correction_T_max  0.3430
_exptl_absorpt_correction_T_min  0.1363
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/2 (Bruker,2014/2) was used for absorption correction.
wR2(int) was 0.1624 before and 0.0629 after correction.
The Ratio of minimum to maximum transmission is 0.3974.
The λ/2 correction factor is Not present.
;
_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    3.129
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1136
_exptl_crystal_preparation       ', Luminescent'
_exptl_crystal_recrystallization_method 
'Slow cool from concentrated HBr solution'
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            44328
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.150
_diffrn_reflns_theta_min         2.538
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4713
_reflns_number_total             5184
_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       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         1.610
_refine_diff_density_min         -1.231
_refine_diff_density_rms         0.177
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     119
_refine_ls_number_reflns         5184
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0222
_refine_ls_R_factor_gt           0.0177
_refine_ls_restrained_S_all      1.067
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0182P)²+0.6817P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0394
_refine_ls_wR_factor_ref         0.0407
_refine_special_details          
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1D,H1E), C2(H2A,H2B)
2.b Aromatic/amide H refined with riding coordinates:
 N3(H3), N2(H2), C5(H5), 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
Pb1 Pb 0.48300(2) 0.77609(2) 0.26029(2) 0.00947(2) Uani 1 1 d . . . . .
Br1 Br 0.77364(2) 0.72689(2) 0.36550(2) 0.01341(4) Uani 1 1 d . . . . .
Br3 Br 0.49844(2) 0.74322(2) 0.02337(2) 0.01643(5) Uani 1 1 d . . . . .
Br4 Br 0.43269(2) 0.52672(2) 0.26154(2) 0.01458(4) Uani 1 1 d . . . . .
Br2 Br 0.18300(2) 0.81139(2) 0.13641(2) 0.01534(5) Uani 1 1 d . . . . .
N1 N 0.7270(2) 0.50563(18) 0.53289(17) 0.0158(4) Uani 1 1 d . . . . .
H1A H 0.6865 0.5674 0.4869 0.019 Uiso 1 1 calc GR . . . .
H1B H 0.6678 0.4712 0.5630 0.019 Uiso 1 1 calc GR . . . .
H1C H 0.7531 0.4534 0.4877 0.019 Uiso 1 1 calc GR . . . .
N3 N 1.1709(2) 0.43965(18) 0.83975(17) 0.0160(4) Uani 1 1 d . . . . .
H3 H 1.1958 0.3832 0.8020 0.019 Uiso 1 1 calc R . . . .
N2 N 1.1781(2) 0.57280(19) 0.96682(18) 0.0200(4) Uani 1 1 d . . . . .
H2 H 1.2086 0.6204 1.0279 0.024 Uiso 1 1 calc R . . . .
C5 C 1.2515(3) 0.4942(2) 0.9360(2) 0.0201(5) Uani 1 1 d . . . . .
H5 H 1.3449 0.4793 0.9754 0.024 Uiso 1 1 calc R . . . .
C1 C 0.8479(2) 0.5464(2) 0.63316(19) 0.0153(4) Uani 1 1 d . . . . .
H1D H 0.8185 0.5957 0.6878 0.018 Uiso 1 1 calc R . . . .
H1E H 0.9057 0.5941 0.6010 0.018 Uiso 1 1 calc R . . . .
C3 C 1.0418(2) 0.4849(2) 0.80786(19) 0.0139(4) Uani 1 1 d . . . . .
C2 C 0.9283(2) 0.4438(2) 0.7016(2) 0.0170(4) Uani 1 1 d . . . . .
H2A H 0.8685 0.3923 0.7277 0.020 Uiso 1 1 calc R . . . .
H2B H 0.9647 0.3984 0.6488 0.020 Uiso 1 1 calc R . . . .
C4 C 1.0473(2) 0.5693(2) 0.8894(2) 0.0185(4) Uani 1 1 d . . . . .
H4 H 0.9746 0.6166 0.8923 0.022 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br1 2.9414(4) . ?
Pb1 Br3 2.9096(4) . ?
Pb1 Br3 3.0934(4) 4_576 ?
Pb1 Br4 2.9179(4) . ?
Pb1 Br4 3.0539(4) 2_655 ?
Pb1 Br2 3.0253(4) . ?
Br3 Pb1 3.0934(4) 4_575 ?
Br4 Pb1 3.0539(4) 2_645 ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 H1C 0.9100 . ?
N1 C1 1.494(3) . ?
N3 H3 0.8800 . ?
N3 C5 1.329(3) . ?
N3 C3 1.383(3) . ?
N2 H2 0.8800 . ?
N2 C5 1.321(3) . ?
N2 C4 1.373(3) . ?
C5 H5 0.9500 . ?
C1 H1D 0.9900 . ?
C1 H1E 0.9900 . ?
C1 C2 1.518(3) . ?
C3 C2 1.491(3) . ?
C3 C4 1.361(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C4 H4 0.9500 . ?

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 82.396(8) . 4_576 ?
Br1 Pb1 Br4 85.809(8) . 2_655 ?
Br1 Pb1 Br2 175.188(7) . . ?
Br3 Pb1 Br1 89.612(9) . . ?
Br3 Pb1 Br3 167.015(6) . 4_576 ?
Br3 Pb1 Br4 85.717(7) . 2_655 ?
Br3 Pb1 Br4 87.011(7) . . ?
Br3 Pb1 Br2 86.533(9) . . ?
Br4 Pb1 Br1 88.472(8) . . ?
Br4 Pb1 Br3 103.788(6) 2_655 4_576 ?
Br4 Pb1 Br3 82.580(6) . 4_576 ?
Br4 Pb1 Br4 170.773(4) . 2_655 ?
Br4 Pb1 Br2 88.453(7) . . ?
Br2 Pb1 Br3 100.870(8) . 4_576 ?
Br2 Pb1 Br4 96.761(8) . 2_655 ?
Pb1 Br3 Pb1 173.261(10) . 4_575 ?
Pb1 Br4 Pb1 150.319(10) . 2_645 ?
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 . . ?
C5 N3 H3 125.1 . . ?
C5 N3 C3 109.8(2) . . ?
C3 N3 H3 125.1 . . ?
C5 N2 H2 125.0 . . ?
C5 N2 C4 110.0(2) . . ?
C4 N2 H2 125.0 . . ?
N3 C5 H5 126.3 . . ?
N2 C5 N3 107.5(2) . . ?
N2 C5 H5 126.3 . . ?
N1 C1 H1D 109.5 . . ?
N1 C1 H1E 109.5 . . ?
N1 C1 C2 110.69(19) . . ?
H1D C1 H1E 108.1 . . ?
C2 C1 H1D 109.5 . . ?
C2 C1 H1E 109.5 . . ?
N3 C3 C2 122.8(2) . . ?
C4 C3 N3 105.9(2) . . ?
C4 C3 C2 131.3(2) . . ?
C1 C2 H2A 109.6 . . ?
C1 C2 H2B 109.6 . . ?
C3 C2 C1 110.4(2) . . ?
C3 C2 H2A 109.6 . . ?
C3 C2 H2B 109.6 . . ?
H2A C2 H2B 108.1 . . ?
N2 C4 H4 126.6 . . ?
C3 C4 N2 106.8(2) . . ?
C3 C4 H4 126.6 . . ?

####################################################################### 
# 
# 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_p21c_2
_database_code_depnum_ccdc_archive 'CCDC 1521059'
_audit_update_record             
;
2016-12-06 deposited with the CCDC.
2017-04-24 downloaded from the CCDC.
;
_audit_creation_date             2015-11-12
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        'octanediammonium tetrabromoplumbate'
_chemical_formula_moiety         '(Br4 Pb1), C8 H22 N2'
_chemical_formula_sum            'C8 H22 Br4 N2 Pb'
_chemical_formula_weight         673.10
_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                   13.807(3)
_cell_length_b                   7.9891(14)
_cell_length_c                   8.2769(14)
_cell_angle_alpha                90
_cell_angle_beta                 104.340(6)
_cell_angle_gamma                90
_cell_volume                     884.5(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6235
_cell_measurement_temperature    298
_cell_measurement_theta_max      30.49
_cell_measurement_theta_min      2.970
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    18.551
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.3635
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/2 (Bruker,2014/2) was used for absorption correction.
wR2(int) was 0.1278 before and 0.0503 after correction.
The Ratio of minimum to maximum transmission is 0.4872.
The λ/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.527
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             612
_exptl_crystal_preparation       ', Luminescent'
_exptl_crystal_recrystallization_method 
'Slow cooling from concentrated hydrobromic acid'
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            12418
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.506
_diffrn_reflns_theta_min         2.970
_diffrn_ambient_temperature      298
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2216
_reflns_number_total             2706
_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       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         1.442
_refine_diff_density_min         -0.754
_refine_diff_density_rms         0.147
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     90
_refine_ls_number_reflns         2706
_refine_ls_number_restraints     68
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0272
_refine_ls_restrained_S_all      1.050
_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)+(0.0393P)²+0.4830P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0694
_refine_ls_wR_factor_ref         0.0732
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H,H,H,H,H) groups
2. Restrained distances
 C1A-C2
 1.54 with sigma of 0.01
 C4A-C3 \\sim C3-C4
 with sigma of 0.02
 C4-C4_$1 \\sim C4A-C4A_$1
 with sigma of 0.02
 C1-N1 \\sim N1-C1A
 with sigma of 0.02
 C1-C2 \\sim C2-C1A
 with sigma of 0.01
3. Rigid bond restraints
 N1, C1, C2, C3, C4, C4A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
N1 \\sim C1 \\sim C2 \\sim C1A: within 2A with sigma of 0.02 and sigma for
terminal atoms of 0.04
N1 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C4A: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08
5. Others
 Sof(H1BD)=Sof(H1BE)=Sof(H1BF)=Sof(H2BC)=Sof(H2BD)=Sof(C1A)=Sof(H1AD)=
 Sof(H1AE)=1-FVAR(1)
 Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H2AA)=Sof(H2AB)=
 FVAR(1)
 Sof(H3BC)=Sof(H3BD)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=1-FVAR(2)
 Sof(H3AA)=Sof(H3AB)=Sof(C4)=Sof(H4A)=Sof(H4B)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2AA,H2AB), C2(H2BC,H2BD), C3(H3AA,H3AB), C3(H3BC,H3BD),
 C4(H4A,H4B), C4A(H4AA,H4AB), C1A(H1AD,H1AE)
6.b Me refined with riding coordinates:
 N1(H1AA,H1AB,H1AC), N1(H1BD,H1BE,H1BF)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.5000 1.0000 0.5000 0.03724(8) Uani 1 2 d S T P . .
Br1 Br 0.53599(4) 0.80948(6) 0.20908(5) 0.05534(13) Uani 1 1 d . . . . .
Br2 Br 0.71947(4) 1.06671(7) 0.61994(7) 0.06226(14) Uani 1 1 d . . . . .
N1 N 0.3093(4) -0.0231(5) 0.9844(7) 0.0636(11) Uani 1 1 d D U . . .
H1AA H 0.3637 0.0343 1.0343 0.076 Uiso 0.261(17) 1 calc R . . A 1
H1AB H 0.3009 -0.1080 1.0492 0.076 Uiso 0.261(17) 1 calc R . . A 1
H1AC H 0.3163 -0.0626 0.8874 0.076 Uiso 0.261(17) 1 calc R . . A 1
H1BD H 0.3681 0.0135 0.9731 0.076 Uiso 0.739(17) 1 calc R . . A 2
H1BE H 0.3028 0.0019 1.0859 0.076 Uiso 0.739(17) 1 calc R . . A 2
H1BF H 0.3058 -0.1336 0.9701 0.076 Uiso 0.739(17) 1 calc R . . A 2
C1 C 0.2196(9) 0.090(2) 0.954(3) 0.070(4) Uani 0.261(17) 1 d D U . A 1
H1A H 0.2127 0.1343 1.0600 0.084 Uiso 0.261(17) 1 calc R . . A 1
H1B H 0.2293 0.1833 0.8852 0.084 Uiso 0.261(17) 1 calc R . . A 1
C2 C 0.1277(6) 0.0002(8) 0.8720(14) 0.109(3) Uani 1 1 d D U . . .
H2AA H 0.0937 -0.0265 0.9581 0.131 Uiso 0.261(17) 1 calc R . . A 1
H2AB H 0.1484 -0.1055 0.8336 0.131 Uiso 0.261(17) 1 calc R . . A 1
H2BC H 0.1158 0.0375 0.9769 0.131 Uiso 0.739(17) 1 calc R . . A 2
H2BD H 0.1247 -0.1210 0.8686 0.131 Uiso 0.739(17) 1 calc R . . A 2
C3 C 0.0501(6) 0.0728(14) 0.7281(11) 0.123(3) Uani 1 1 d D U . . .
H3AA H 0.0674 0.1874 0.7087 0.148 Uiso 0.591(19) 1 calc R . . B 1
H3AB H -0.0145 0.0734 0.7548 0.148 Uiso 0.591(19) 1 calc R . . B 1
H3BC H 0.0498 0.1896 0.7598 0.148 Uiso 0.409(19) 1 calc R . . B 2
H3BD H -0.0113 0.0274 0.7474 0.148 Uiso 0.409(19) 1 calc R . . B 2
C4 C 0.0440(8) -0.031(2) 0.5711(15) 0.088(4) Uani 0.591(19) 1 d D U . B 1
H4A H 0.0341 -0.1481 0.5942 0.106 Uiso 0.591(19) 1 calc R . . B 1
H4B H 0.1061 -0.0214 0.5372 0.106 Uiso 0.591(19) 1 calc R . . B 1
C4A C 0.0244(15) 0.0844(19) 0.5354(19) 0.097(6) Uani 0.409(19) 1 d D U . B 2
H4AA H 0.0845 0.1041 0.4978 0.116 Uiso 0.409(19) 1 calc R . . B 2
H4AB H -0.0217 0.1761 0.4973 0.116 Uiso 0.409(19) 1 calc R . . B 2
C1A C 0.2275(5) 0.0585(12) 0.8571(14) 0.076(3) Uani 0.739(17) 1 d D U . A 2
H1AD H 0.2320 0.1790 0.8716 0.092 Uiso 0.739(17) 1 calc R . . A 2
H1AE H 0.2352 0.0327 0.7465 0.092 Uiso 0.739(17) 1 calc R . . A 2


_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 2.9881(6) 4_576 ?
Pb1 Br1 2.9924(5) . ?
Pb1 Br1 2.9881(6) 2_655 ?
Pb1 Br1 2.9924(5) 3_676 ?
Pb1 Br2 2.9936(7) . ?
Pb1 Br2 2.9936(7) 3_676 ?
Br1 Pb1 2.9881(6) 2_645 ?
N1 H1AA 0.8900 . ?
N1 H1AB 0.8900 . ?
N1 H1AC 0.8900 . ?
N1 H1BD 0.8900 . ?
N1 H1BE 0.8900 . ?
N1 H1BF 0.8900 . ?
N1 C1 1.502(15) . ?
N1 C1A 1.490(9) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C2 1.469(12) . ?
C2 H2AA 0.9700 . ?
C2 H2AB 0.9700 . ?
C2 H2BC 0.9700 . ?
C2 H2BD 0.9700 . ?
C2 C3 1.507(12) . ?
C2 C1A 1.487(8) . ?
C3 H3AA 0.9700 . ?
C3 H3AB 0.9700 . ?
C3 H3BC 0.9700 . ?
C3 H3BD 0.9700 . ?
C3 C4 1.527(14) . ?
C3 C4A 1.548(16) . ?
C4 C4 1.55(2) 3_556 ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4A C4A 1.56(2) 3_556 ?
C4A H4AA 0.9700 . ?
C4A H4AB 0.9700 . ?
C1A H1AD 0.9700 . ?
C1A H1AE 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br1 Pb1 Br1 180.0 4_576 2_655 ?
Br1 Pb1 Br1 90.471(13) 4_576 . ?
Br1 Pb1 Br1 89.529(13) 2_655 . ?
Br1 Pb1 Br1 90.471(13) 2_655 3_676 ?
Br1 Pb1 Br1 89.529(13) 4_576 3_676 ?
Br1 Pb1 Br1 180.0 3_676 . ?
Br1 Pb1 Br2 89.929(16) . 3_676 ?
Br1 Pb1 Br2 86.892(16) 2_655 3_676 ?
Br1 Pb1 Br2 93.108(15) 4_576 3_676 ?
Br1 Pb1 Br2 90.071(16) 3_676 3_676 ?
Br1 Pb1 Br2 90.070(16) . . ?
Br1 Pb1 Br2 86.892(15) 4_576 . ?
Br1 Pb1 Br2 93.108(15) 2_655 . ?
Br1 Pb1 Br2 89.930(16) 3_676 . ?
Br2 Pb1 Br2 180.0 3_676 . ?
Pb1 Br1 Pb1 148.208(18) 2_645 . ?
H1AA N1 H1AB 109.5 . . ?
H1AA N1 H1AC 109.5 . . ?
H1AB N1 H1AC 109.5 . . ?
H1BD N1 H1BE 109.5 . . ?
H1BD N1 H1BF 109.5 . . ?
H1BE N1 H1BF 109.5 . . ?
C1 N1 H1AA 109.5 . . ?
C1 N1 H1AB 109.5 . . ?
C1 N1 H1AC 109.5 . . ?
C1A N1 H1BD 109.5 . . ?
C1A N1 H1BE 109.5 . . ?
C1A N1 H1BF 109.5 . . ?
N1 C1 H1A 109.3 . . ?
N1 C1 H1B 109.3 . . ?
H1A C1 H1B 108.0 . . ?
C2 C1 N1 111.4(10) . . ?
C2 C1 H1A 109.3 . . ?
C2 C1 H1B 109.3 . . ?
C1 C2 H2AA 106.6 . . ?
C1 C2 H2AB 106.6 . . ?
C1 C2 C3 122.9(11) . . ?
H2AA C2 H2AB 106.6 . . ?
H2BC C2 H2BD 108.4 . . ?
C3 C2 H2AA 106.6 . . ?
C3 C2 H2AB 106.6 . . ?
C3 C2 H2BC 110.1 . . ?
C3 C2 H2BD 110.1 . . ?
C1A C2 H2BC 110.1 . . ?
C1A C2 H2BD 110.1 . . ?
C1A C2 C3 107.9(8) . . ?
C2 C3 H3AA 109.7 . . ?
C2 C3 H3AB 109.7 . . ?
C2 C3 H3BC 101.9 . . ?
C2 C3 H3BD 101.9 . . ?
C2 C3 C4 110.0(7) . . ?
C2 C3 C4A 140.7(11) . . ?
H3AA C3 H3AB 108.2 . . ?
H3BC C3 H3BD 104.7 . . ?
C4 C3 H3AA 109.7 . . ?
C4 C3 H3AB 109.7 . . ?
C4A C3 H3BC 101.9 . . ?
C4A C3 H3BD 101.9 . . ?
C3 C4 C4 109.8(11) . 3_556 ?
C3 C4 H4A 109.7 . . ?
C3 C4 H4B 109.7 . . ?
C4 C4 H4A 109.7 3_556 . ?
C4 C4 H4B 109.7 3_556 . ?
H4A C4 H4B 108.2 . . ?
C3 C4A C4A 107.7(15) . 3_556 ?
C3 C4A H4AA 110.2 . . ?
C3 C4A H4AB 110.2 . . ?
C4A C4A H4AA 110.2 3_556 . ?
C4A C4A H4AB 110.2 3_556 . ?
H4AA C4A H4AB 108.5 . . ?
N1 C1A H1AD 109.4 . . ?
N1 C1A H1AE 109.4 . . ?
C2 C1A N1 111.1(7) . . ?
C2 C1A H1AD 109.4 . . ?
C2 C1A H1AE 109.4 . . ?
H1AD C1A H1AE 108.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 -135.7(13) . . . . ?
N1 C1 C2 C1A -63.0(12) . . . . ?
C1 N1 C1A C2 -62.3(10) . . . . ?
C1 C2 C3 C4 115.0(15) . . . . ?
C1 C2 C3 C4A 87.8(19) . . . . ?
C1 C2 C1A N1 63.6(12) . . . . ?
C2 C3 C4 C4 173.6(14) . . . 3_556 ?
C2 C3 C4A C4A 79(3) . . . 3_556 ?
C3 C2 C1A N1 -173.7(8) . . . . ?
C4 C3 C4A C4A 34.2(12) . . . 3_556 ?
C4A C3 C4 C4 -34.9(12) . . . 3_556 ?
C1A N1 C1 C2 64.0(10) . . . . ?
C1A C2 C3 C4 80.5(12) . . . . ?
C1A C2 C3 C4A 53.3(18) . . . . ?

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

data_g1_p21c_0p83_a
_database_code_depnum_ccdc_archive 'CCDC 1521055'
_audit_update_record             
;
2016-12-06 deposited with the CCDC.
2017-04-24 downloaded from the CCDC.
;
_audit_creation_date             2015-12-16
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        
'3-(2-ammonioethyl)-anilinium tetrabromoplumbate'
_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 0.0040 0.0020 '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 -0.7410 2.7890 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0080 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -6.2900 11.6060 '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                   7.7688(3)
_cell_length_b                   8.5108(4)
_cell_length_c                   24.6314(11)
_cell_angle_alpha                90
_cell_angle_beta                 95.197(2)
_cell_angle_gamma                90
_cell_volume                     1621.90(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9887
_cell_measurement_temperature    298
_cell_measurement_theta_max      31.52
_cell_measurement_theta_min      2.76
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    24.973
_exptl_absorpt_correction_T_max  0.2999
_exptl_absorpt_correction_T_min  0.0924
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/2 (Bruker,2014/2) was used for absorption correction.
wR2(int) was 0.1698 before and 0.1064 after correction.
The Ratio of minimum to maximum transmission is 0.3081.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.724
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1192
_exptl_crystal_preparation       ', Luminescent'
_exptl_crystal_recrystallization_method 'Slow-cooled from concentrated HBr'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.01
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0889
_diffrn_reflns_av_unetI/netI     0.0436
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            32430
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         27.833
_diffrn_reflns_theta_min         2.609
_diffrn_ambient_temperature      298
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           ?
_diffrn_radiation_wavelength     0.7749
_diffrn_source                   ?
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2659
_reflns_number_total             3017
_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       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         4.194
_refine_diff_density_min         -2.671
_refine_diff_density_rms         0.432
_refine_ls_extinction_coef       0.0019(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         3017
_refine_ls_number_restraints     83
_refine_ls_R_factor_all          0.0780
_refine_ls_R_factor_gt           0.0710
_refine_ls_restrained_S_all      1.109
_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)+(0.0960P)²+64.7434P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2031
_refine_ls_wR_factor_ref         0.2092
_refine_special_details          'Refined as a 2-component twin., Twin'
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.9664(13) 0.0336(13)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
3. Restrained distances
 C2-C1
 1.54 with sigma of 0.02
4. Rigid bond restraints
 N2, N1, C5, C6, C4, C7, C3, C8, C1, C2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
N2 \\sim N1 \\sim C5 \\sim C6 \\sim C4 \\sim C7 \\sim C3 \\sim C8 \\sim C1
\\sim C2: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
6.a Secondary CH2 refined with riding coordinates:
 C1(H1D,H1E), C2(H2D,H2E)
6.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C4(H4), C7(H7), C8(H8)
6.c Idealised Me refined as rotating group:
 N2(H2A,H2B,H2C), 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
Pb1 Pb 0.74591(8) 0.30986(9) 0.74641(3) 0.0319(3) Uani 1 1 d . . . . .
Br3 Br 0.4273(3) 0.5017(3) 0.72604(9) 0.0511(6) Uani 1 1 d . . . . .
Br4 Br 0.9355(3) 0.6102(3) 0.73384(12) 0.0634(7) Uani 1 1 d . . . . .
Br2 Br 0.7542(4) 0.3907(3) 0.86463(9) 0.0592(7) Uani 1 1 d . . . . .
Br1 Br 0.7391(4) 0.2313(3) 0.62847(9) 0.0608(7) Uani 1 1 d . . . . .
N2 N 0.174(3) 0.270(2) 0.6362(7) 0.052(4) Uani 1 1 d . U . . .
H2A H 0.2103 0.1707 0.6366 0.063 Uiso 1 1 calc GR . . . .
H2B H 0.0616 0.2724 0.6403 0.063 Uiso 1 1 calc GR . . . .
H2C H 0.2315 0.3226 0.6633 0.063 Uiso 1 1 calc GR . . . .
N1 N 0.317(3) 0.150(3) 0.3517(8) 0.071(6) Uani 1 1 d . U . . .
H1A H 0.2671 0.1789 0.3193 0.085 Uiso 1 1 calc GR . . . .
H1B H 0.2857 0.0525 0.3591 0.085 Uiso 1 1 calc GR . . . .
H1C H 0.4315 0.1545 0.3513 0.085 Uiso 1 1 calc GR . . . .
C5 C 0.205(3) 0.341(2) 0.5850(9) 0.046(4) Uani 1 1 d . U . . .
C6 C 0.195(3) 0.500(3) 0.5793(9) 0.054(5) Uani 1 1 d . U . . .
H6 H 0.1675 0.5632 0.6080 0.064 Uiso 1 1 calc R . . . .
C4 C 0.235(4) 0.246(3) 0.5419(9) 0.060(6) Uani 1 1 d . U . . .
H4 H 0.2310 0.1375 0.5459 0.072 Uiso 1 1 calc R . . . .
C7 C 0.226(4) 0.563(3) 0.5304(10) 0.070(6) Uani 1 1 d . U . . .
H7 H 0.2212 0.6711 0.5264 0.085 Uiso 1 1 calc R . . . .
C3 C 0.271(5) 0.310(3) 0.4925(10) 0.073(6) Uani 1 1 d . U . . .
C8 C 0.262(4) 0.475(3) 0.4879(10) 0.073(7) Uani 1 1 d . U . . .
H8 H 0.2816 0.5228 0.4551 0.088 Uiso 1 1 calc R . . . .
C1 C 0.262(5) 0.258(4) 0.3943(9) 0.089(9) Uani 1 1 d D U . . .
H1D H 0.1371 0.2592 0.3929 0.106 Uiso 1 1 calc R . . . .
H1E H 0.3002 0.3642 0.3869 0.106 Uiso 1 1 calc R . . . .
C2 C 0.336(5) 0.210(4) 0.4503(9) 0.097(9) Uani 1 1 d D U . . .
H2D H 0.3050 0.1018 0.4567 0.117 Uiso 1 1 calc R . . . .
H2E H 0.4607 0.2173 0.4525 0.117 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br3 2.970(2) . ?
Pb1 Br3 3.052(2) 2_646 ?
Pb1 Br4 3.005(2) 2_746 ?
Pb1 Br4 2.980(2) . ?
Pb1 Br2 2.987(2) . ?
Pb1 Br1 2.977(2) . ?
Br3 Pb1 3.052(2) 2_656 ?
Br4 Pb1 3.005(2) 2_756 ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 H2C 0.8900 . ?
N2 C5 1.44(3) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C1 1.49(3) . ?
C5 C6 1.36(3) . ?
C5 C4 1.37(3) . ?
C6 H6 0.9300 . ?
C6 C7 1.36(3) . ?
C4 H4 0.9300 . ?
C4 C3 1.39(3) . ?
C7 H7 0.9300 . ?
C7 C8 1.34(4) . ?
C3 C8 1.41(3) . ?
C3 C2 1.47(4) . ?
C8 H8 0.9300 . ?
C1 H1D 0.9700 . ?
C1 H1E 0.9700 . ?
C1 C2 1.500(18) . ?
C2 H2D 0.9700 . ?
C2 H2E 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br3 Pb1 Br3 97.61(3) . 2_646 ?
Br3 Pb1 Br4 85.59(7) . . ?
Br3 Pb1 Br4 178.88(8) . 2_746 ?
Br3 Pb1 Br2 88.98(7) . . ?
Br3 Pb1 Br1 91.01(7) . . ?
Br4 Pb1 Br3 172.81(7) . 2_646 ?
Br4 Pb1 Br3 81.45(7) 2_746 2_646 ?
Br4 Pb1 Br4 95.41(3) . 2_746 ?
Br4 Pb1 Br2 86.37(8) . . ?
Br2 Pb1 Br3 87.26(7) . 2_646 ?
Br2 Pb1 Br4 91.59(8) . 2_746 ?
Br1 Pb1 Br3 93.13(7) . 2_646 ?
Br1 Pb1 Br4 88.43(8) . 2_746 ?
Br1 Pb1 Br4 93.24(8) . . ?
Br1 Pb1 Br2 179.61(8) . . ?
Pb1 Br3 Pb1 144.33(9) . 2_656 ?
Pb1 Br4 Pb1 151.13(10) . 2_756 ?
H2A N2 H2B 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
C5 N2 H2A 109.5 . . ?
C5 N2 H2B 109.5 . . ?
C5 N2 H2C 109.5 . . ?
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 . . ?
C6 C5 N2 120(2) . . ?
C6 C5 C4 121(2) . . ?
C4 C5 N2 118.8(19) . . ?
C5 C6 H6 121.0 . . ?
C5 C6 C7 118(2) . . ?
C7 C6 H6 121.0 . . ?
C5 C4 H4 119.7 . . ?
C5 C4 C3 121(2) . . ?
C3 C4 H4 119.7 . . ?
C6 C7 H7 118.6 . . ?
C8 C7 C6 123(2) . . ?
C8 C7 H7 118.6 . . ?
C4 C3 C8 117(2) . . ?
C4 C3 C2 120(2) . . ?
C8 C3 C2 122(2) . . ?
C7 C8 C3 120(2) . . ?
C7 C8 H8 119.8 . . ?
C3 C8 H8 119.8 . . ?
N1 C1 H1D 109.3 . . ?
N1 C1 H1E 109.3 . . ?
N1 C1 C2 112(2) . . ?
H1D C1 H1E 107.9 . . ?
C2 C1 H1D 109.3 . . ?
C2 C1 H1E 109.3 . . ?
C3 C2 C1 112(2) . . ?
C3 C2 H2D 109.3 . . ?
C3 C2 H2E 109.3 . . ?
C1 C2 H2D 109.3 . . ?
C1 C2 H2E 109.3 . . ?
H2D C2 H2E 108.0 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.9664(13)
2 0.0336(13)

####################################################################### 
# 
# 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_aj80_p21c_a
_database_code_depnum_ccdc_archive 'CCDC 1521060'
_audit_update_record             
;
2016-12-06 deposited with the CCDC.
2017-04-24 downloaded from the CCDC.
;
_audit_creation_date             2015-11-04
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        
'bis(4-ammoniobutanoic acid) tetrabromoplumbate'
_chemical_formula_moiety         '0.5(Br24 Pb6), 6(C4 H10 N O2)'
_chemical_formula_sum            'C24 H60 Br12 N6 O12 Pb3'
_chemical_formula_weight         2205.27
_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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           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                   24.7721(12)
_cell_length_b                   8.0709(4)
_cell_length_c                   56.964(3)
_cell_angle_alpha                90
_cell_angle_beta                 97.137(2)
_cell_angle_gamma                90
_cell_volume                     11300.6(10)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9300
_cell_measurement_temperature    298
_cell_measurement_theta_max      25.815
_cell_measurement_theta_min      2.409
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    17.452
_exptl_absorpt_correction_T_max  0.4296
_exptl_absorpt_correction_T_min  0.2782
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/2 (Bruker,2014/2) was used for absorption correction.
wR2(int) was 0.0964 before and 0.0608 after correction.
The Ratio of minimum to maximum transmission is 0.6476.
The λ/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.592
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             8064
_exptl_crystal_preparation       ', Luminescent'
_exptl_crystal_recrystallization_method 'from HBr'
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1030
_diffrn_reflns_av_unetI/netI     0.0694
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       70
_diffrn_reflns_limit_l_min       -70
_diffrn_reflns_number            205643
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         2.057
_diffrn_ambient_temperature      298
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                12004
_reflns_number_total             22216
_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       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         1.907
_refine_diff_density_min         -1.615
_refine_diff_density_rms         0.194
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1053
_refine_ls_number_reflns         22216
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1251
_refine_ls_R_factor_gt           0.0493
_refine_ls_restrained_S_all      1.013
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0257P)²+47.8012P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0757
_refine_ls_wR_factor_ref         0.0928
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C45(H45A,H45B), C34(H34A,H34B), C37(H37A,H37B), C6(H6D,H6E),
 C29(H29A,H29B), C1(H1D,H1E), C17(H17A,H17B), C26(H26A,H26B), C2(H2A,H2B),
 C41(H41A,H41B), C25(H25A,H25B), C46(H46A,H46B), C5(H5D,H5E), C31(H31A,H31),
 C18(H18A,H18B), C35(H35A,H35), C30(H30A,H30B), C3(H3A,H3B), C22(H22A,H22B),
 C27(H27A,H27B), C10(H10D,H10E), C47(H47A,H47B), C21(H21A,H21B), C7(H7D,H7E),
 C9(H9D,H9E), C11(H11D,H11E), C15(H15A,H15B), C19(H19A,H19B), C42(H42A,H42B),
 C39(H39A,H39B), C38(H38A,H38B), C43(H43A,H43B), C23(H23A,H23B), C14(H14A,H14B),
  C13(H13A,H13B)
2.b Tetrahedral OH refined with riding coordinates:
 O22(H22)
2.c Idealised Me refined as rotating group:
 N8(H8A,H8B,H8C), N7(H7A,H7B,H7C), N10(H10A,H10B,H10C), N9(H9A,H9B,H9C),
 N1(H1A,H1B,H1C), N5(H5A,H5B,H5C), N6(H6A,H6B,H6C), N11(H11A,H11B,H11C),
 N12(H12A,H12B,H12C), N4(H4A,H4B,H4C), N2(H2C,H2D,H2E), N3(H3C,H3D,H3E)
2.d Idealised tetrahedral OH refined as rotating group:
 O12(H12), O10(H10), O5(H5), O16(H16), O17(H17), O24(H24), O3(H3), O19(H19),
 O7(H7), O13(H13), O2(H2)
;
_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
Pb3 Pb 0.08419(2) 1.41540(4) 0.24716(2) 0.03111(10) Uani 1 1 d . . . . .
Pb2 Pb 0.25090(2) 0.92973(4) 0.24376(2) 0.03101(10) Uani 1 1 d . . . . .
Pb1 Pb 0.41633(2) 1.41564(5) 0.24744(2) 0.03166(10) Uani 1 1 d . . . . .
Pb5 Pb 0.33294(2) 0.98956(4) 0.50603(2) 0.02944(10) Uani 1 1 d . . . . .
Pb6 Pb 0.16683(2) 0.50485(5) 0.50356(2) 0.03087(10) Uani 1 1 d . . . . .
Pb4 Pb 0.5000 0.5000 0.5000 0.02948(14) Uani 1 2 d S T P . .
Pb7 Pb 0.0000 1.0000 0.5000 0.03313(14) Uani 1 2 d S T P . .
Br13 Br 0.47798(4) 1.10222(13) 0.23941(2) 0.0473(3) Uani 1 1 d . . . . .
Br20 Br 0.18439(4) 1.62562(13) 0.25252(2) 0.0470(3) Uani 1 1 d . . . . .
Br4 Br 0.40003(4) 0.28925(13) 0.49676(2) 0.0487(3) Uani 1 1 d . . . . .
Br16 Br 0.41098(5) 1.34038(13) 0.29896(2) 0.0504(3) Uani 1 1 d . . . . .
Br7 Br 0.23198(4) 1.19706(13) 0.49648(2) 0.0481(3) Uani 1 1 d . . . . .
Br6 Br 0.43744(4) 0.79781(13) 0.51263(2) 0.0502(3) Uani 1 1 d . . . . .
Br1 Br 0.32439(4) 0.91591(13) 0.45503(2) 0.0477(3) Uani 1 1 d . . . . .
Br22 Br 0.25586(5) 1.00291(14) 0.29474(2) 0.0505(3) Uani 1 1 d . . . . .
Br14 Br 0.35224(4) 0.72557(14) 0.25330(2) 0.0540(3) Uani 1 1 d . . . . .
Br18 Br 0.07279(5) 1.49018(14) 0.19577(2) 0.0509(3) Uani 1 1 d . . . . .
Br11 Br 0.10591(4) 0.81713(13) 0.51141(2) 0.0505(3) Uani 1 1 d . . . . .
Br24 Br 0.14422(4) 1.11229(14) 0.23542(2) 0.0550(3) Uani 1 1 d . . . . .
Br15 Br 0.42174(5) 1.48880(14) 0.19675(2) 0.0537(3) Uani 1 1 d . . . . .
Br23 Br 0.24925(5) 0.85733(14) 0.19250(2) 0.0509(3) Uani 1 1 d . . . . .
Br3 Br 0.33868(5) 1.07105(14) 0.55740(2) 0.0494(3) Uani 1 1 d . . . . .
Br17 Br 0.30994(5) 1.24189(14) 0.23558(2) 0.0569(3) Uani 1 1 d . . . . .
Br5 Br 0.51850(5) 0.43033(13) 0.55181(2) 0.0514(3) Uani 1 1 d . . . . .
Br9 Br 0.06270(4) 1.31169(14) 0.49243(2) 0.0535(3) Uani 1 1 d . . . . .
Br21 Br 0.09961(5) 1.34265(14) 0.29916(2) 0.0525(3) Uani 1 1 d . . . . .
Br19 Br 0.01897(4) 1.71482(14) 0.25842(2) 0.0524(3) Uani 1 1 d . . . . .
Br8 Br 0.17001(5) 0.58113(13) 0.45184(2) 0.0504(3) Uani 1 1 d . . . . .
Br2 Br 0.27380(5) 0.68017(14) 0.51572(2) 0.0557(3) Uani 1 1 d . . . . .
Br10 Br 0.16377(5) 0.43249(14) 0.55423(2) 0.0514(3) Uani 1 1 d . . . . .
Br12 Br 0.00373(5) 0.92896(14) 0.44885(2) 0.0540(3) Uani 1 1 d . . . . .
N8 N 0.1209(4) 0.9344(11) 0.29145(16) 0.055(3) Uani 1 1 d . . . . .
H8A H 0.1126 1.0351 0.2963 0.066 Uiso 1 1 calc GR . . . .
H8B H 0.0939 0.8969 0.2810 0.066 Uiso 1 1 calc GR . . . .
H8C H 0.1514 0.9393 0.2847 0.066 Uiso 1 1 calc GR . . . .
N7 N -0.2130(3) 0.9549(11) 0.30111(16) 0.057(3) Uani 1 1 d . . . . .
H7A H -0.2181 1.0580 0.3059 0.069 Uiso 1 1 calc GR . . . .
H7B H -0.2404 0.9262 0.2903 0.069 Uiso 1 1 calc GR . . . .
H7C H -0.1819 0.9491 0.2949 0.069 Uiso 1 1 calc GR . . . .
N10 N 0.2739(4) 0.4125(11) 0.29146(17) 0.060(3) Uani 1 1 d . . . . .
H10A H 0.2598 0.4587 0.2779 0.071 Uiso 1 1 calc GR . . . .
H10B H 0.2600 0.3117 0.2926 0.071 Uiso 1 1 calc GR . . . .
H10C H 0.3099 0.4052 0.2918 0.071 Uiso 1 1 calc GR . . . .
N9 N 0.4406(3) 0.9341(10) 0.29242(16) 0.055(3) Uani 1 1 d . . . . .
H9A H 0.4155 0.9071 0.2805 0.066 Uiso 1 1 calc GR . . . .
H9B H 0.4730 0.9404 0.2873 0.066 Uiso 1 1 calc GR . . . .
H9C H 0.4323 1.0317 0.2983 0.066 Uiso 1 1 calc GR . . . .
N1 N 0.4593(3) 0.9798(10) 0.45643(16) 0.054(3) Uani 1 1 d . . . . .
H1A H 0.4830 1.0272 0.4674 0.064 Uiso 1 1 calc GR . . . .
H1B H 0.4721 0.8819 0.4525 0.064 Uiso 1 1 calc GR . . . .
H1C H 0.4277 0.9656 0.4621 0.064 Uiso 1 1 calc GR . . . .
N5 N 0.6118(4) 0.3912(12) 0.30194(18) 0.069(3) Uani 1 1 d . . . . .
H5A H 0.5970 0.2928 0.3042 0.083 Uiso 1 1 calc GR . . . .
H5B H 0.6449 0.3770 0.2978 0.083 Uiso 1 1 calc GR . . . .
H5C H 0.5911 0.4450 0.2905 0.083 Uiso 1 1 calc GR . . . .
N6 N -0.0407(4) 0.3899(11) 0.29750(17) 0.060(3) Uani 1 1 d . . . . .
H6A H -0.0505 0.2870 0.3007 0.072 Uiso 1 1 calc GR . . . .
H6B H -0.0099 0.3875 0.2910 0.072 Uiso 1 1 calc GR . . . .
H6C H -0.0667 0.4365 0.2874 0.072 Uiso 1 1 calc GR . . . .
N11 N 0.3077(3) 0.5062(10) 0.45935(16) 0.055(3) Uani 1 1 d . . . . .
H11A H 0.3218 0.6070 0.4582 0.066 Uiso 1 1 calc GR . . . .
H11B H 0.3224 0.4590 0.4728 0.066 Uiso 1 1 calc GR . . . .
H11C H 0.2719 0.5141 0.4593 0.066 Uiso 1 1 calc GR . . . .
O1 O 0.5762(3) 1.0875(11) 0.38968(15) 0.065(2) Uani 1 1 d . . . . .
O18 O 0.3096(3) 0.8572(10) 0.35305(14) 0.060(2) Uani 1 1 d . . . . .
O12 O -0.1709(4) 0.2758(11) 0.36372(17) 0.076(3) Uani 1 1 d . . . . .
H12 H -0.1935 0.3042 0.3723 0.113 Uiso 1 1 calc GR . . . .
N12 N 0.1413(3) 0.9857(10) 0.45862(16) 0.052(3) Uani 1 1 d . . . . .
H12A H 0.1545 0.8914 0.4536 0.063 Uiso 1 1 calc GR . . . .
H12B H 0.1080 0.9682 0.4625 0.063 Uiso 1 1 calc GR . . . .
H12C H 0.1629 1.0222 0.4712 0.063 Uiso 1 1 calc GR . . . .
O23 O 0.2689(3) 1.0659(10) 0.39678(14) 0.063(2) Uani 1 1 d . . . . .
N4 N -0.0255(4) 0.5266(11) 0.45183(19) 0.070(3) Uani 1 1 d . . . . .
H4A H -0.0041 0.4716 0.4629 0.083 Uiso 1 1 calc GR . . . .
H4B H -0.0585 0.5376 0.4563 0.083 Uiso 1 1 calc GR . . . .
H4C H -0.0115 0.6263 0.4498 0.083 Uiso 1 1 calc GR . . . .
O10 O 0.4652(3) 0.2887(10) 0.36435(16) 0.066(2) Uani 1 1 d . . . . .
H10 H 0.4402 0.3219 0.3713 0.100 Uiso 1 1 calc GR . . . .
O5 O -0.2367(4) 0.6310(11) 0.38652(18) 0.083(3) Uani 1 1 d . . . . .
H5 H -0.2124 0.6032 0.3788 0.125 Uiso 1 1 calc GR . . . .
O16 O 0.0060(4) 0.8337(11) 0.35807(16) 0.068(3) Uani 1 1 d . . . . .
H16 H -0.0119 0.8454 0.3691 0.102 Uiso 1 1 calc GR . . . .
O17 O 0.3564(3) 1.0511(11) 0.37387(18) 0.080(3) Uani 1 1 d . . . . .
H17 H 0.3277 1.0618 0.3795 0.120 Uiso 1 1 calc GR . . . .
N2 N -0.1996(3) 0.9723(10) 0.45015(17) 0.059(3) Uani 1 1 d . . . . .
H2C H -0.1742 1.0010 0.4619 0.071 Uiso 1 1 calc GR . . . .
H2D H -0.1926 0.8709 0.4452 0.071 Uiso 1 1 calc GR . . . .
H2E H -0.2321 0.9736 0.4553 0.071 Uiso 1 1 calc GR . . . .
N3 N -0.3771(4) 0.5311(10) 0.44885(17) 0.058(3) Uani 1 1 d . . . . .
H3C H -0.3540 0.4797 0.4597 0.069 Uiso 1 1 calc GR . . . .
H3D H -0.4092 0.5418 0.4541 0.069 Uiso 1 1 calc GR . . . .
H3E H -0.3641 0.6309 0.4460 0.069 Uiso 1 1 calc GR . . . .
O14 O -0.3487(3) 0.8323(10) 0.36050(14) 0.062(2) Uani 1 1 d . . . . .
O24 O 0.2223(3) 0.8725(11) 0.37570(16) 0.073(3) Uani 1 1 d . . . . .
H24 H 0.2476 0.8066 0.3764 0.110 Uiso 1 1 calc GR . . . .
O3 O -0.0620(4) 1.0847(11) 0.39128(17) 0.071(3) Uani 1 1 d . . . . .
H3 H -0.0357 1.0674 0.3842 0.106 Uiso 1 1 calc GR . . . .
O20 O 0.3873(4) 0.3971(11) 0.39073(16) 0.075(3) Uani 1 1 d . . . . .
C33 C 0.4421(4) 0.8073(13) 0.31093(19) 0.046(3) Uani 1 1 d . . . . .
H33A H 0.4746 0.8229 0.3221 0.055 Uiso 1 1 calc R . . . .
H33B H 0.4444 0.6989 0.3038 0.055 Uiso 1 1 calc R . . . .
O19 O 0.4056(4) 0.6605(10) 0.38644(16) 0.069(2) Uani 1 1 d . . . . .
H19 H 0.4334 0.6230 0.3820 0.104 Uiso 1 1 calc GR . . . .
O9 O 0.4786(4) 0.5575(12) 0.36006(16) 0.079(3) Uani 1 1 d . . . . .
O11 O -0.1598(4) 0.5472(14) 0.36100(17) 0.090(4) Uani 1 1 d . . . . .
O21 O 0.1906(4) 0.5240(12) 0.35883(17) 0.088(3) Uani 1 1 d . . . . .
O6 O -0.2465(4) 0.3595(13) 0.38981(16) 0.080(3) Uani 1 1 d . . . . .
O7 O 0.1139(4) 0.6361(10) 0.38609(17) 0.077(3) Uani 1 1 d . . . . .
H7 H 0.1333 0.6039 0.3763 0.115 Uiso 1 1 calc GR . . . .
C45 C 0.1385(4) 1.1135(13) 0.4392(2) 0.052(3) Uani 1 1 d . . . . .
H45A H 0.1063 1.0933 0.4281 0.063 Uiso 1 1 calc R . . . .
H45B H 0.1349 1.2224 0.4460 0.063 Uiso 1 1 calc R . . . .
C34 C 0.3936(4) 0.8121(12) 0.32398(18) 0.043(3) Uani 1 1 d . . . . .
H34A H 0.3612 0.8252 0.3127 0.051 Uiso 1 1 calc R . . . .
H34B H 0.3907 0.7070 0.3320 0.051 Uiso 1 1 calc R . . . .
O22 O 0.1707(4) 0.2628(10) 0.36336(16) 0.085(3) Uani 1 1 d . . . . .
H22 H 0.1504 0.3016 0.3723 0.127 Uiso 1 1 calc R . . . .
O15 O 0.0206(4) 1.0950(13) 0.36531(19) 0.107(4) Uani 1 1 d . . . . .
C37 C 0.2605(6) 0.5182(13) 0.3119(2) 0.066(4) Uani 1 1 d . . . . .
H37A H 0.2752 0.6285 0.3104 0.079 Uiso 1 1 calc R . . . .
H37B H 0.2213 0.5282 0.3111 0.079 Uiso 1 1 calc R . . . .
C6 C -0.1450(4) 1.0930(13) 0.4204(2) 0.053(3) Uani 1 1 d . . . . .
H6D H -0.1436 1.1917 0.4108 0.064 Uiso 1 1 calc R . . . .
H6E H -0.1157 1.1001 0.4333 0.064 Uiso 1 1 calc R . . . .
C29 C 0.1288(5) 0.8222(14) 0.3118(2) 0.061(3) Uani 1 1 d . . . . .
H29A H 0.1611 0.8566 0.3221 0.073 Uiso 1 1 calc R . . . .
H29B H 0.1354 0.7115 0.3062 0.073 Uiso 1 1 calc R . . . .
C36 C 0.3497(5) 0.9441(14) 0.3563(2) 0.047(3) Uani 1 1 d . . . . .
C48 C 0.2302(5) 0.9749(15) 0.3935(2) 0.048(3) Uani 1 1 d . . . . .
C28 C -0.3264(5) 0.9621(18) 0.3575(2) 0.050(3) Uani 1 1 d . . . . .
C32 C 0.0324(5) 0.9596(19) 0.3558(2) 0.058(4) Uani 1 1 d . . . . .
C1 C 0.4508(5) 1.0888(14) 0.4349(2) 0.064(4) Uani 1 1 d . . . . .
H1D H 0.4200 1.0475 0.4244 0.076 Uiso 1 1 calc R . . . .
H1E H 0.4420 1.1998 0.4398 0.076 Uiso 1 1 calc R . . . .
C17 C 0.6155(5) 0.4871(16) 0.3237(3) 0.079(4) Uani 1 1 d . . . . .
H17A H 0.6312 0.5945 0.3210 0.095 Uiso 1 1 calc R . . . .
H17B H 0.6398 0.4308 0.3358 0.095 Uiso 1 1 calc R . . . .
C26 C -0.2646(5) 0.8292(15) 0.3312(2) 0.063(4) Uani 1 1 d . . . . .
H26A H -0.2932 0.8119 0.3182 0.076 Uiso 1 1 calc R . . . .
H26B H -0.2639 0.7336 0.3416 0.076 Uiso 1 1 calc R . . . .
C12 C -0.2606(5) 0.500(2) 0.3935(2) 0.058(4) Uani 1 1 d . . . . .
C2 C 0.4989(5) 1.0974(14) 0.4219(2) 0.062(4) Uani 1 1 d . . . . .
H2A H 0.4943 1.1904 0.4110 0.075 Uiso 1 1 calc R . . . .
H2B H 0.5309 1.1191 0.4331 0.075 Uiso 1 1 calc R . . . .
C41 C 0.3200(5) 0.4001(13) 0.4382(2) 0.063(4) Uani 1 1 d . . . . .
H41A H 0.3591 0.3918 0.4383 0.076 Uiso 1 1 calc R . . . .
H41B H 0.3059 0.2891 0.4399 0.076 Uiso 1 1 calc R . . . .
C25 C -0.2109(5) 0.8408(16) 0.3215(2) 0.069(4) Uani 1 1 d . . . . .
H25A H -0.1833 0.8789 0.3339 0.083 Uiso 1 1 calc R . . . .
H25B H -0.2004 0.7314 0.3167 0.083 Uiso 1 1 calc R . . . .
O13 O -0.3426(4) 1.1030(12) 0.3645(2) 0.095(3) Uani 1 1 d . . . . .
H13 H -0.3635 1.0884 0.3744 0.143 Uiso 1 1 calc GR . . . .
O4 O -0.0754(4) 0.8216(13) 0.3833(2) 0.121(5) Uani 1 1 d . . . . .
C8 C -0.0874(5) 0.955(2) 0.3927(2) 0.057(4) Uani 1 1 d . . . . .
C46 C 0.1863(4) 1.1136(12) 0.42623(19) 0.048(3) Uani 1 1 d . . . . .
H46A H 0.2190 1.1037 0.4374 0.057 Uiso 1 1 calc R . . . .
H46B H 0.1880 1.2185 0.4180 0.057 Uiso 1 1 calc R . . . .
C5 C -0.1992(4) 1.0901(14) 0.4306(2) 0.059(3) Uani 1 1 d . . . . .
H5D H -0.2068 1.2002 0.4361 0.071 Uiso 1 1 calc R . . . .
H5E H -0.2279 1.0609 0.4181 0.071 Uiso 1 1 calc R . . . .
O8 O 0.0994(4) 0.3688(13) 0.39018(19) 0.103(4) Uani 1 1 d . . . . .
C24 C -0.1471(5) 0.406(2) 0.3565(2) 0.068(4) Uani 1 1 d . . . . .
C4 C 0.5545(5) 0.9593(18) 0.3934(2) 0.054(4) Uani 1 1 d . . . . .
C31 C 0.0759(4) 0.9637(14) 0.3403(2) 0.058(3) Uani 1 1 d . . . . .
H31A H 0.0692 1.0572 0.3296 0.070 Uiso 1 1 calc R . . . .
H31 H 0.1102 0.9843 0.3501 0.070 Uiso 1 1 calc R . . . .
C18 C 0.5617(5) 0.5120(14) 0.3324(2) 0.072(4) Uani 1 1 d . . . . .
H18A H 0.5653 0.6033 0.3436 0.086 Uiso 1 1 calc R . . . .
H18B H 0.5358 0.5460 0.3191 0.086 Uiso 1 1 calc R . . . .
C35 C 0.3954(5) 0.9473(13) 0.3416(2) 0.053(3) Uani 1 1 d . . . . .
H35A H 0.3949 1.0527 0.3334 0.063 Uiso 1 1 calc R . . . .
H35 H 0.4295 0.9403 0.3520 0.063 Uiso 1 1 calc R . . . .
O2 O 0.5689(4) 0.8150(11) 0.38627(19) 0.091(3) Uani 1 1 d . . . . .
H2 H 0.5916 0.8267 0.3771 0.136 Uiso 1 1 calc GR . . . .
C30 C 0.0823(5) 0.8154(13) 0.3260(2) 0.059(3) Uani 1 1 d . . . . .
H30A H 0.0490 0.7983 0.3154 0.071 Uiso 1 1 calc R . . . .
H30B H 0.0871 0.7203 0.3365 0.071 Uiso 1 1 calc R . . . .
C3 C 0.5088(5) 0.9462(15) 0.4083(2) 0.066(4) Uani 1 1 d . . . . .
H3A H 0.4758 0.9190 0.3980 0.079 Uiso 1 1 calc R . . . .
H3B H 0.5166 0.8552 0.4193 0.079 Uiso 1 1 calc R . . . .
C16 C 0.0879(6) 0.512(2) 0.3935(2) 0.071(4) Uani 1 1 d . . . . .
C20 C 0.4916(5) 0.4146(18) 0.3572(2) 0.056(3) Uani 1 1 d . . . . .
C40 C 0.2003(5) 0.3819(17) 0.3558(2) 0.060(4) Uani 1 1 d . . . . .
C22 C -0.0813(6) 0.5116(16) 0.3308(2) 0.087(5) Uani 1 1 d . . . . .
H22A H -0.0734 0.5964 0.3428 0.104 Uiso 1 1 calc R . . . .
H22B H -0.1097 0.5544 0.3191 0.104 Uiso 1 1 calc R . . . .
C27 C -0.2773(5) 0.9752(16) 0.3443(2) 0.072(4) Uani 1 1 d . . . . .
H27A H -0.2831 1.0671 0.3333 0.087 Uiso 1 1 calc R . . . .
H27B H -0.2459 1.0021 0.3556 0.087 Uiso 1 1 calc R . . . .
C44 C 0.3770(6) 0.5392(18) 0.3940(2) 0.064(4) Uani 1 1 d . . . . .
C10 C -0.3322(5) 0.3994(15) 0.4164(3) 0.082(5) Uani 1 1 d . . . . .
H10D H -0.3057 0.3501 0.4284 0.099 Uiso 1 1 calc R . . . .
H10E H -0.3403 0.3185 0.4039 0.099 Uiso 1 1 calc R . . . .
C47 C 0.1849(5) 0.9745(14) 0.4085(2) 0.061(4) Uani 1 1 d . . . . .
H47A H 0.1856 0.8701 0.4170 0.074 Uiso 1 1 calc R . . . .
H47B H 0.1506 0.9800 0.3982 0.074 Uiso 1 1 calc R . . . .
C21 C -0.0328(5) 0.4860(17) 0.3193(3) 0.089(5) Uani 1 1 d . . . . .
H21A H -0.0058 0.4305 0.3303 0.107 Uiso 1 1 calc R . . . .
H21B H -0.0182 0.5935 0.3158 0.107 Uiso 1 1 calc R . . . .
C7 C -0.1360(5) 0.9470(14) 0.4059(2) 0.064(4) Uani 1 1 d . . . . .
H7D H -0.1680 0.9306 0.3945 0.077 Uiso 1 1 calc R . . . .
H7E H -0.1323 0.8505 0.4161 0.077 Uiso 1 1 calc R . . . .
C9 C -0.3834(5) 0.4349(16) 0.4272(2) 0.078(4) Uani 1 1 d . . . . .
H9D H -0.4084 0.4932 0.4156 0.093 Uiso 1 1 calc R . . . .
H9E H -0.4002 0.3300 0.4304 0.093 Uiso 1 1 calc R . . . .
C11 C -0.3079(5) 0.5433(15) 0.4068(2) 0.077(4) Uani 1 1 d . . . . .
H11D H -0.2954 0.6184 0.4196 0.093 Uiso 1 1 calc R . . . .
H11E H -0.3354 0.6005 0.3962 0.093 Uiso 1 1 calc R . . . .
C15 C 0.0433(5) 0.5597(16) 0.4067(2) 0.075(4) Uani 1 1 d . . . . .
H15A H 0.0146 0.6101 0.3959 0.090 Uiso 1 1 calc R . . . .
H15B H 0.0564 0.6421 0.4184 0.090 Uiso 1 1 calc R . . . .
C19 C 0.5380(5) 0.3691(14) 0.3440(2) 0.065(4) Uani 1 1 d . . . . .
H19A H 0.5663 0.3178 0.3550 0.078 Uiso 1 1 calc R . . . .
H19B H 0.5256 0.2876 0.3321 0.078 Uiso 1 1 calc R . . . .
C42 C 0.2963(5) 0.4682(16) 0.4158(2) 0.074(4) Uani 1 1 d . . . . .
H42A H 0.2610 0.5148 0.4178 0.089 Uiso 1 1 calc R . . . .
H42B H 0.2903 0.3786 0.4044 0.089 Uiso 1 1 calc R . . . .
C39 C 0.2480(6) 0.3208(15) 0.3446(2) 0.078(4) Uani 1 1 d . . . . .
H39A H 0.2348 0.2453 0.3319 0.094 Uiso 1 1 calc R . . . .
H39B H 0.2713 0.2578 0.3563 0.094 Uiso 1 1 calc R . . . .
C38 C 0.2818(6) 0.4514(17) 0.3347(3) 0.084(4) Uani 1 1 d . . . . .
H38A H 0.2868 0.5421 0.3459 0.101 Uiso 1 1 calc R . . . .
H38B H 0.3175 0.4050 0.3334 0.101 Uiso 1 1 calc R . . . .
C43 C 0.3297(5) 0.5994(15) 0.4058(2) 0.075(4) Uani 1 1 d . . . . .
H43A H 0.3435 0.6740 0.4185 0.090 Uiso 1 1 calc R . . . .
H43B H 0.3060 0.6633 0.3943 0.090 Uiso 1 1 calc R . . . .
C23 C -0.1025(5) 0.3682(17) 0.3418(3) 0.084(5) Uani 1 1 d . . . . .
H23A H -0.0729 0.3151 0.3518 0.101 Uiso 1 1 calc R . . . .
H23B H -0.1161 0.2900 0.3296 0.101 Uiso 1 1 calc R . . . .
C14 C 0.0203(6) 0.4156(18) 0.4189(3) 0.105(6) Uani 1 1 d . . . . .
H14A H 0.0145 0.3264 0.4074 0.126 Uiso 1 1 calc R . . . .
H14B H 0.0481 0.3785 0.4312 0.126 Uiso 1 1 calc R . . . .
C13 C -0.0296(6) 0.4346(18) 0.4295(3) 0.097(5) Uani 1 1 d . . . . .
H13A H -0.0437 0.3250 0.4322 0.117 Uiso 1 1 calc R . . . .
H13B H -0.0561 0.4900 0.4182 0.117 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb3 Br20 2.9908(10) . ?
Pb3 Br18 2.9678(12) . ?
Pb3 Br24 2.9816(11) . ?
Pb3 Br21 2.9975(12) . ?
Pb3 Br19 3.0084(11) 2_545 ?
Pb3 Br19 3.0198(11) . ?
Pb2 Br20 3.0318(11) 1_545 ?
Pb2 Br22 2.9510(12) . ?
Pb2 Br14 2.9956(11) . ?
Pb2 Br24 3.0114(11) . ?
Pb2 Br23 2.9731(12) . ?
Pb2 Br17 2.9789(11) . ?
Pb1 Br13 3.0191(11) . ?
Pb1 Br13 3.0325(11) 2_655 ?
Pb1 Br16 3.0158(12) . ?
Pb1 Br14 3.0034(11) 1_565 ?
Pb1 Br15 2.9666(12) . ?
Pb1 Br17 2.9876(11) . ?
Pb5 Br4 3.0183(10) 1_565 ?
Pb5 Br7 3.0029(11) . ?
Pb5 Br6 2.9992(10) . ?
Pb5 Br1 2.9471(12) . ?
Pb5 Br3 2.9856(12) . ?
Pb5 Br2 2.9812(11) . ?
Pb6 Br7 3.0166(11) 1_545 ?
Pb6 Br11 2.9997(11) . ?
Pb6 Br9 3.0135(11) 1_545 ?
Pb6 Br8 3.0206(12) . ?
Pb6 Br2 3.0078(11) . ?
Pb6 Br10 2.9551(12) . ?
Pb4 Br4 2.9910(10) . ?
Pb4 Br4 2.9910(10) 3_666 ?
Pb4 Br6 2.9956(10) 3_666 ?
Pb4 Br6 2.9956(10) . ?
Pb4 Br5 2.9834(12) 3_666 ?
Pb4 Br5 2.9833(12) . ?
Pb7 Br11 3.0100(10) 3_576 ?
Pb7 Br11 3.0100(10) . ?
Pb7 Br9 3.0154(10) 3_576 ?
Pb7 Br9 3.0154(10) . ?
Pb7 Br12 2.9824(12) . ?
Pb7 Br12 2.9822(12) 3_576 ?
Br13 Pb1 3.0326(11) 2_645 ?
Br20 Pb2 3.0318(10) 1_565 ?
Br4 Pb5 3.0181(10) 1_545 ?
Br7 Pb6 3.0167(11) 1_565 ?
Br14 Pb1 3.0034(11) 1_545 ?
Br9 Pb6 3.0135(11) 1_565 ?
Br19 Pb3 3.0085(11) 2 ?
N8 H8A 0.8900 . ?
N8 H8B 0.8900 . ?
N8 H8C 0.8900 . ?
N8 C29 1.466(13) . ?
N7 H7A 0.8900 . ?
N7 H7B 0.8900 . ?
N7 H7C 0.8900 . ?
N7 C25 1.479(13) . ?
N10 H10A 0.8900 . ?
N10 H10B 0.8900 . ?
N10 H10C 0.8900 . ?
N10 C37 1.514(14) . ?
N9 H9A 0.8900 . ?
N9 H9B 0.8900 . ?
N9 H9C 0.8900 . ?
N9 C33 1.466(12) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C1 1.501(13) . ?
N5 H5A 0.8900 . ?
N5 H5B 0.8900 . ?
N5 H5C 0.8900 . ?
N5 C17 1.454(14) . ?
N6 H6A 0.8900 . ?
N6 H6B 0.8900 . ?
N6 H6C 0.8900 . ?
N6 C21 1.456(15) . ?
N11 H11A 0.8900 . ?
N11 H11B 0.8900 . ?
N11 H11C 0.8900 . ?
N11 C41 1.539(14) . ?
O1 C4 1.197(13) . ?
O18 C36 1.213(12) . ?
O12 H12 0.8200 . ?
O12 C24 1.298(15) . ?
N12 H12A 0.8900 . ?
N12 H12B 0.8900 . ?
N12 H12C 0.8900 . ?
N12 C45 1.509(12) . ?
O23 C48 1.204(13) . ?
N4 H4A 0.8900 . ?
N4 H4B 0.8900 . ?
N4 H4C 0.8900 . ?
N4 C13 1.465(15) . ?
O10 H10 0.8200 . ?
O10 C20 1.300(14) . ?
O5 H5 0.8200 . ?
O5 C12 1.300(14) . ?
O16 H16 0.8200 . ?
O16 C32 1.224(13) . ?
O17 H17 0.8200 . ?
O17 C36 1.317(13) . ?
N2 H2C 0.8900 . ?
N2 H2D 0.8900 . ?
N2 H2E 0.8900 . ?
N2 C5 1.467(13) . ?
N3 H3C 0.8900 . ?
N3 H3D 0.8900 . ?
N3 H3E 0.8900 . ?
N3 C9 1.449(14) . ?
O14 C28 1.205(13) . ?
O24 H24 0.8200 . ?
O24 C48 1.306(13) . ?
O3 H3 0.8200 . ?
O3 C8 1.227(13) . ?
O20 C44 1.193(13) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C33 C34 1.491(12) . ?
O19 H19 0.8200 . ?
O19 C44 1.312(13) . ?
O9 C20 1.213(13) . ?
O11 C24 1.218(15) . ?
O21 C40 1.189(12) . ?
O6 C12 1.209(13) . ?
O7 H7 0.8200 . ?
O7 C16 1.289(14) . ?
C45 H45A 0.9700 . ?
C45 H45B 0.9700 . ?
C45 C46 1.470(13) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C34 C35 1.480(13) . ?
O22 H22 0.8200 . ?
O22 C40 1.313(13) . ?
O15 C32 1.270(14) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C37 C38 1.441(16) . ?
C6 H6D 0.9700 . ?
C6 H6E 0.9700 . ?
C6 C5 1.528(14) . ?
C6 C7 1.472(14) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C29 C30 1.490(14) . ?
C36 C35 1.489(14) . ?
C48 C47 1.492(14) . ?
C28 O13 1.285(13) . ?
C28 C27 1.513(15) . ?
C32 C31 1.477(15) . ?
C1 H1D 0.9700 . ?
C1 H1E 0.9700 . ?
C1 C2 1.482(14) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 C18 1.493(14) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C26 C25 1.505(14) . ?
C26 C27 1.449(15) . ?
C12 C11 1.514(16) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C3 1.482(14) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C41 C42 1.445(16) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
O13 H13 0.8200 . ?
O4 C8 1.257(14) . ?
C8 C7 1.496(15) . ?
C46 H46A 0.9700 . ?
C46 H46B 0.9700 . ?
C46 C47 1.506(14) . ?
C5 H5D 0.9700 . ?
C5 H5E 0.9700 . ?
O8 C16 1.210(14) . ?
C24 C23 1.495(17) . ?
C4 O2 1.297(13) . ?
C4 C3 1.499(15) . ?
C31 H31A 0.9700 . ?
C31 H31 0.9700 . ?
C31 C30 1.465(14) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 C19 1.486(15) . ?
C35 H35A 0.9700 . ?
C35 H35 0.9700 . ?
O2 H2 0.8200 . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C16 C15 1.465(17) . ?
C20 C19 1.496(16) . ?
C40 C39 1.495(16) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 C21 1.453(15) . ?
C22 C23 1.446(16) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C44 C43 1.502(16) . ?
C10 H10D 0.9700 . ?
C10 H10E 0.9700 . ?
C10 C9 1.506(15) . ?
C10 C11 1.446(15) . ?
C47 H47A 0.9700 . ?
C47 H47B 0.9700 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C7 H7D 0.9700 . ?
C7 H7E 0.9700 . ?
C9 H9D 0.9700 . ?
C9 H9E 0.9700 . ?
C11 H11D 0.9700 . ?
C11 H11E 0.9700 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 C14 1.503(17) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C42 C43 1.501(15) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C39 C38 1.500(16) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C13 1.450(16) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br20 Pb3 Br21 90.46(3) . . ?
Br20 Pb3 Br19 177.99(3) . 2_545 ?
Br20 Pb3 Br19 89.05(3) . . ?
Br18 Pb3 Br20 87.79(3) . . ?
Br18 Pb3 Br24 86.26(3) . . ?
Br18 Pb3 Br21 178.11(3) . . ?
Br18 Pb3 Br19 93.38(3) . . ?
Br18 Pb3 Br19 91.70(3) . 2_545 ?
Br24 Pb3 Br20 93.30(3) . . ?
Br24 Pb3 Br21 93.15(3) . . ?
Br24 Pb3 Br19 88.60(3) . 2_545 ?
Br24 Pb3 Br19 177.60(4) . . ?
Br21 Pb3 Br19 90.07(3) . 2_545 ?
Br21 Pb3 Br19 87.29(3) . . ?
Br19 Pb3 Br19 89.038(15) 2_545 . ?
Br22 Pb2 Br20 87.54(3) . 1_545 ?
Br22 Pb2 Br14 90.00(3) . . ?
Br22 Pb2 Br24 89.18(3) . . ?
Br22 Pb2 Br23 178.39(3) . . ?
Br22 Pb2 Br17 91.34(3) . . ?
Br14 Pb2 Br20 89.15(3) . 1_545 ?
Br14 Pb2 Br24 175.54(4) . . ?
Br24 Pb2 Br20 86.44(3) . 1_545 ?
Br23 Pb2 Br20 93.51(3) . 1_545 ?
Br23 Pb2 Br14 88.80(3) . . ?
Br23 Pb2 Br24 92.10(3) . . ?
Br23 Pb2 Br17 87.69(3) . . ?
Br17 Pb2 Br20 176.27(3) . 1_545 ?
Br17 Pb2 Br14 94.41(3) . . ?
Br17 Pb2 Br24 89.99(3) . . ?
Br13 Pb1 Br13 90.917(16) . 2_655 ?
Br16 Pb1 Br13 90.03(3) . 2_655 ?
Br16 Pb1 Br13 93.61(3) . . ?
Br14 Pb1 Br13 90.63(3) 1_565 2_655 ?
Br14 Pb1 Br13 177.47(4) 1_565 . ?
Br14 Pb1 Br16 88.39(3) 1_565 . ?
Br15 Pb1 Br13 89.97(3) . 2_655 ?
Br15 Pb1 Br13 86.23(3) . . ?
Br15 Pb1 Br16 179.84(4) . . ?
Br15 Pb1 Br14 91.77(3) . 1_565 ?
Br15 Pb1 Br17 91.06(4) . . ?
Br17 Pb1 Br13 91.21(3) . . ?
Br17 Pb1 Br13 177.69(4) . 2_655 ?
Br17 Pb1 Br16 88.94(3) . . ?
Br17 Pb1 Br14 87.28(3) . 1_565 ?
Br7 Pb5 Br4 89.18(3) . 1_565 ?
Br6 Pb5 Br4 87.14(3) . 1_565 ?
Br6 Pb5 Br7 175.50(3) . . ?
Br1 Pb5 Br4 87.87(3) . 1_565 ?
Br1 Pb5 Br7 88.72(3) . . ?
Br1 Pb5 Br6 88.55(3) . . ?
Br1 Pb5 Br3 178.25(3) . . ?
Br1 Pb5 Br2 92.11(3) . . ?
Br3 Pb5 Br4 92.00(3) . 1_565 ?
Br3 Pb5 Br7 89.53(3) . . ?
Br3 Pb5 Br6 93.18(3) . . ?
Br2 Pb5 Br4 176.04(3) . 1_565 ?
Br2 Pb5 Br7 94.77(3) . . ?
Br2 Pb5 Br6 88.91(3) . . ?
Br2 Pb5 Br3 88.15(3) . . ?
Br7 Pb6 Br8 87.60(3) 1_545 . ?
Br11 Pb6 Br7 177.85(4) . 1_545 ?
Br11 Pb6 Br9 91.87(3) . 1_545 ?
Br11 Pb6 Br8 92.79(3) . . ?
Br11 Pb6 Br2 90.89(3) . . ?
Br9 Pb6 Br7 90.23(3) 1_545 1_545 ?
Br9 Pb6 Br8 91.46(3) 1_545 . ?
Br2 Pb6 Br7 86.99(3) . 1_545 ?
Br2 Pb6 Br9 176.82(4) . 1_545 ?
Br2 Pb6 Br8 89.98(3) . . ?
Br10 Pb6 Br7 92.69(3) . 1_545 ?
Br10 Pb6 Br11 86.90(3) . . ?
Br10 Pb6 Br9 88.75(3) . 1_545 ?
Br10 Pb6 Br8 179.64(4) . . ?
Br10 Pb6 Br2 89.82(3) . . ?
Br4 Pb4 Br4 180.0 3_666 . ?
Br4 Pb4 Br6 91.26(3) . . ?
Br4 Pb4 Br6 88.74(3) 3_666 . ?
Br4 Pb4 Br6 91.26(3) 3_666 3_666 ?
Br4 Pb4 Br6 88.74(3) . 3_666 ?
Br6 Pb4 Br6 180.0 3_666 . ?
Br5 Pb4 Br4 91.25(3) . 3_666 ?
Br5 Pb4 Br4 91.25(3) 3_666 . ?
Br5 Pb4 Br4 88.75(3) . . ?
Br5 Pb4 Br4 88.75(3) 3_666 3_666 ?
Br5 Pb4 Br6 93.78(3) 3_666 . ?
Br5 Pb4 Br6 86.22(3) . . ?
Br5 Pb4 Br6 93.77(3) . 3_666 ?
Br5 Pb4 Br6 86.23(3) 3_666 3_666 ?
Br5 Pb4 Br5 180.0 . 3_666 ?
Br11 Pb7 Br11 180.0 . 3_576 ?
Br11 Pb7 Br9 90.61(3) . 3_576 ?
Br11 Pb7 Br9 89.39(3) 3_576 3_576 ?
Br11 Pb7 Br9 90.61(3) 3_576 . ?
Br11 Pb7 Br9 89.39(3) . . ?
Br9 Pb7 Br9 180.0 3_576 . ?
Br12 Pb7 Br11 89.13(3) . . ?
Br12 Pb7 Br11 90.87(3) . 3_576 ?
Br12 Pb7 Br11 90.87(3) 3_576 . ?
Br12 Pb7 Br11 89.13(3) 3_576 3_576 ?
Br12 Pb7 Br9 93.34(3) . 3_576 ?
Br12 Pb7 Br9 86.65(3) . . ?
Br12 Pb7 Br9 93.35(3) 3_576 . ?
Br12 Pb7 Br9 86.66(3) 3_576 3_576 ?
Br12 Pb7 Br12 180.0 3_576 . ?
Pb1 Br13 Pb1 144.69(4) . 2_645 ?
Pb3 Br20 Pb2 154.62(4) . 1_565 ?
Pb4 Br4 Pb5 156.15(4) . 1_545 ?
Pb5 Br7 Pb6 151.93(4) . 1_565 ?
Pb4 Br6 Pb5 148.01(4) . . ?
Pb2 Br14 Pb1 151.71(5) . 1_545 ?
Pb6 Br11 Pb7 145.18(4) . . ?
Pb3 Br24 Pb2 144.93(5) . . ?
Pb2 Br17 Pb1 142.95(5) . . ?
Pb6 Br9 Pb7 147.58(5) 1_565 . ?
Pb3 Br19 Pb3 151.41(5) 2 . ?
Pb5 Br2 Pb6 142.24(5) . . ?
H8A N8 H8B 109.5 . . ?
H8A N8 H8C 109.5 . . ?
H8B N8 H8C 109.5 . . ?
C29 N8 H8A 109.5 . . ?
C29 N8 H8B 109.5 . . ?
C29 N8 H8C 109.5 . . ?
H7A N7 H7B 109.5 . . ?
H7A N7 H7C 109.5 . . ?
H7B N7 H7C 109.5 . . ?
C25 N7 H7A 109.5 . . ?
C25 N7 H7B 109.5 . . ?
C25 N7 H7C 109.5 . . ?
H10A N10 H10B 109.5 . . ?
H10A N10 H10C 109.5 . . ?
H10B N10 H10C 109.5 . . ?
C37 N10 H10A 109.5 . . ?
C37 N10 H10B 109.5 . . ?
C37 N10 H10C 109.5 . . ?
H9A N9 H9B 109.5 . . ?
H9A N9 H9C 109.5 . . ?
H9B N9 H9C 109.5 . . ?
C33 N9 H9A 109.5 . . ?
C33 N9 H9B 109.5 . . ?
C33 N9 H9C 109.5 . . ?
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 . . ?
H5A N5 H5B 109.5 . . ?
H5A N5 H5C 109.5 . . ?
H5B N5 H5C 109.5 . . ?
C17 N5 H5A 109.5 . . ?
C17 N5 H5B 109.5 . . ?
C17 N5 H5C 109.5 . . ?
H6A N6 H6B 109.5 . . ?
H6A N6 H6C 109.5 . . ?
H6B N6 H6C 109.5 . . ?
C21 N6 H6A 109.5 . . ?
C21 N6 H6B 109.5 . . ?
C21 N6 H6C 109.5 . . ?
H11A N11 H11B 109.5 . . ?
H11A N11 H11C 109.5 . . ?
H11B N11 H11C 109.5 . . ?
C41 N11 H11A 109.5 . . ?
C41 N11 H11B 109.5 . . ?
C41 N11 H11C 109.5 . . ?
C24 O12 H12 109.5 . . ?
H12A N12 H12B 109.5 . . ?
H12A N12 H12C 109.5 . . ?
H12B N12 H12C 109.5 . . ?
C45 N12 H12A 109.5 . . ?
C45 N12 H12B 109.5 . . ?
C45 N12 H12C 109.5 . . ?
H4A N4 H4B 109.5 . . ?
H4A N4 H4C 109.5 . . ?
H4B N4 H4C 109.5 . . ?
C13 N4 H4A 109.5 . . ?
C13 N4 H4B 109.5 . . ?
C13 N4 H4C 109.5 . . ?
C20 O10 H10 109.5 . . ?
C12 O5 H5 109.5 . . ?
C32 O16 H16 109.5 . . ?
C36 O17 H17 109.5 . . ?
H2C N2 H2D 109.5 . . ?
H2C N2 H2E 109.5 . . ?
H2D N2 H2E 109.5 . . ?
C5 N2 H2C 109.5 . . ?
C5 N2 H2D 109.5 . . ?
C5 N2 H2E 109.5 . . ?
H3C N3 H3D 109.5 . . ?
H3C N3 H3E 109.5 . . ?
H3D N3 H3E 109.5 . . ?
C9 N3 H3C 109.5 . . ?
C9 N3 H3D 109.5 . . ?
C9 N3 H3E 109.5 . . ?
C48 O24 H24 109.5 . . ?
C8 O3 H3 109.5 . . ?
N9 C33 H33A 109.0 . . ?
N9 C33 H33B 109.0 . . ?
N9 C33 C34 112.9(9) . . ?
H33A C33 H33B 107.8 . . ?
C34 C33 H33A 109.0 . . ?
C34 C33 H33B 109.0 . . ?
C44 O19 H19 109.5 . . ?
C16 O7 H7 109.5 . . ?
N12 C45 H45A 108.8 . . ?
N12 C45 H45B 108.8 . . ?
H45A C45 H45B 107.7 . . ?
C46 C45 N12 113.8(9) . . ?
C46 C45 H45A 108.8 . . ?
C46 C45 H45B 108.8 . . ?
C33 C34 H34A 108.9 . . ?
C33 C34 H34B 108.9 . . ?
H34A C34 H34B 107.7 . . ?
C35 C34 C33 113.5(9) . . ?
C35 C34 H34A 108.9 . . ?
C35 C34 H34B 108.9 . . ?
C40 O22 H22 109.5 . . ?
N10 C37 H37A 109.0 . . ?
N10 C37 H37B 109.0 . . ?
H37A C37 H37B 107.8 . . ?
C38 C37 N10 112.9(10) . . ?
C38 C37 H37A 109.0 . . ?
C38 C37 H37B 109.0 . . ?
H6D C6 H6E 107.7 . . ?
C5 C6 H6D 108.8 . . ?
C5 C6 H6E 108.8 . . ?
C7 C6 H6D 108.8 . . ?
C7 C6 H6E 108.8 . . ?
C7 C6 C5 113.7(10) . . ?
N8 C29 H29A 108.6 . . ?
N8 C29 H29B 108.6 . . ?
N8 C29 C30 114.7(10) . . ?
H29A C29 H29B 107.6 . . ?
C30 C29 H29A 108.6 . . ?
C30 C29 H29B 108.6 . . ?
O18 C36 O17 121.2(11) . . ?
O18 C36 C35 126.3(10) . . ?
O17 C36 C35 112.5(10) . . ?
O23 C48 O24 122.9(11) . . ?
O23 C48 C47 123.7(11) . . ?
O24 C48 C47 113.2(11) . . ?
O14 C28 O13 124.1(12) . . ?
O14 C28 C27 122.8(12) . . ?
O13 C28 C27 113.1(12) . . ?
O16 C32 O15 121.0(12) . . ?
O16 C32 C31 121.4(13) . . ?
O15 C32 C31 117.4(12) . . ?
N1 C1 H1D 108.9 . . ?
N1 C1 H1E 108.9 . . ?
H1D C1 H1E 107.7 . . ?
C2 C1 N1 113.4(9) . . ?
C2 C1 H1D 108.9 . . ?
C2 C1 H1E 108.9 . . ?
N5 C17 H17A 109.0 . . ?
N5 C17 H17B 109.0 . . ?
N5 C17 C18 113.0(11) . . ?
H17A C17 H17B 107.8 . . ?
C18 C17 H17A 109.0 . . ?
C18 C17 H17B 109.0 . . ?
H26A C26 H26B 107.7 . . ?
C25 C26 H26A 108.9 . . ?
C25 C26 H26B 108.9 . . ?
C27 C26 H26A 108.9 . . ?
C27 C26 H26B 108.9 . . ?
C27 C26 C25 113.4(11) . . ?
O5 C12 C11 111.9(13) . . ?
O6 C12 O5 123.9(13) . . ?
O6 C12 C11 124.2(13) . . ?
C1 C2 H2A 108.5 . . ?
C1 C2 H2B 108.5 . . ?
H2A C2 H2B 107.5 . . ?
C3 C2 C1 114.9(10) . . ?
C3 C2 H2A 108.5 . . ?
C3 C2 H2B 108.5 . . ?
N11 C41 H41A 109.1 . . ?
N11 C41 H41B 109.1 . . ?
H41A C41 H41B 107.9 . . ?
C42 C41 N11 112.4(10) . . ?
C42 C41 H41A 109.1 . . ?
C42 C41 H41B 109.1 . . ?
N7 C25 C26 112.3(9) . . ?
N7 C25 H25A 109.1 . . ?
N7 C25 H25B 109.1 . . ?
C26 C25 H25A 109.1 . . ?
C26 C25 H25B 109.1 . . ?
H25A C25 H25B 107.9 . . ?
C28 O13 H13 109.5 . . ?
O3 C8 O4 123.5(12) . . ?
O3 C8 C7 121.5(13) . . ?
O4 C8 C7 115.0(12) . . ?
C45 C46 H46A 109.1 . . ?
C45 C46 H46B 109.1 . . ?
C45 C46 C47 112.4(9) . . ?
H46A C46 H46B 107.8 . . ?
C47 C46 H46A 109.1 . . ?
C47 C46 H46B 109.1 . . ?
N2 C5 C6 112.8(9) . . ?
N2 C5 H5D 109.0 . . ?
N2 C5 H5E 109.0 . . ?
C6 C5 H5D 109.0 . . ?
C6 C5 H5E 109.0 . . ?
H5D C5 H5E 107.8 . . ?
O12 C24 C23 114.1(14) . . ?
O11 C24 O12 123.4(14) . . ?
O11 C24 C23 122.5(14) . . ?
O1 C4 O2 125.1(12) . . ?
O1 C4 C3 123.1(12) . . ?
O2 C4 C3 111.7(12) . . ?
C32 C31 H31A 108.1 . . ?
C32 C31 H31 108.1 . . ?
H31A C31 H31 107.3 . . ?
C30 C31 C32 116.7(10) . . ?
C30 C31 H31A 108.1 . . ?
C30 C31 H31 108.1 . . ?
C17 C18 H18A 107.9 . . ?
C17 C18 H18B 107.9 . . ?
H18A C18 H18B 107.2 . . ?
C19 C18 C17 117.5(11) . . ?
C19 C18 H18A 107.9 . . ?
C19 C18 H18B 107.9 . . ?
C34 C35 C36 114.0(9) . . ?
C34 C35 H35A 108.8 . . ?
C34 C35 H35 108.8 . . ?
C36 C35 H35A 108.8 . . ?
C36 C35 H35 108.8 . . ?
H35A C35 H35 107.7 . . ?
C4 O2 H2 109.5 . . ?
C29 C30 H30A 108.6 . . ?
C29 C30 H30B 108.6 . . ?
C31 C30 C29 114.5(10) . . ?
C31 C30 H30A 108.6 . . ?
C31 C30 H30B 108.6 . . ?
H30A C30 H30B 107.6 . . ?
C2 C3 C4 115.1(10) . . ?
C2 C3 H3A 108.5 . . ?
C2 C3 H3B 108.5 . . ?
C4 C3 H3A 108.5 . . ?
C4 C3 H3B 108.5 . . ?
H3A C3 H3B 107.5 . . ?
O7 C16 C15 113.8(13) . . ?
O8 C16 O7 123.8(13) . . ?
O8 C16 C15 122.5(13) . . ?
O10 C20 C19 114.3(12) . . ?
O9 C20 O10 123.3(12) . . ?
O9 C20 C19 122.2(12) . . ?
O21 C40 O22 121.8(13) . . ?
O21 C40 C39 124.4(12) . . ?
O22 C40 C39 113.7(12) . . ?
H22A C22 H22B 107.3 . . ?
C21 C22 H22A 108.1 . . ?
C21 C22 H22B 108.1 . . ?
C23 C22 H22A 108.1 . . ?
C23 C22 H22B 108.1 . . ?
C23 C22 C21 116.6(12) . . ?
C28 C27 H27A 108.3 . . ?
C28 C27 H27B 108.3 . . ?
C26 C27 C28 116.0(11) . . ?
C26 C27 H27A 108.3 . . ?
C26 C27 H27B 108.3 . . ?
H27A C27 H27B 107.4 . . ?
O20 C44 O19 122.1(13) . . ?
O20 C44 C43 125.0(12) . . ?
O19 C44 C43 112.8(12) . . ?
H10D C10 H10E 107.6 . . ?
C9 C10 H10D 108.7 . . ?
C9 C10 H10E 108.7 . . ?
C11 C10 H10D 108.7 . . ?
C11 C10 H10E 108.7 . . ?
C11 C10 C9 114.4(11) . . ?
C48 C47 C46 115.1(10) . . ?
C48 C47 H47A 108.5 . . ?
C48 C47 H47B 108.5 . . ?
C46 C47 H47A 108.5 . . ?
C46 C47 H47B 108.5 . . ?
H47A C47 H47B 107.5 . . ?
N6 C21 H21A 108.4 . . ?
N6 C21 H21B 108.4 . . ?
C22 C21 N6 115.4(11) . . ?
C22 C21 H21A 108.4 . . ?
C22 C21 H21B 108.4 . . ?
H21A C21 H21B 107.5 . . ?
C6 C7 C8 115.6(10) . . ?
C6 C7 H7D 108.4 . . ?
C6 C7 H7E 108.4 . . ?
C8 C7 H7D 108.4 . . ?
C8 C7 H7E 108.4 . . ?
H7D C7 H7E 107.4 . . ?
N3 C9 C10 116.3(11) . . ?
N3 C9 H9D 108.2 . . ?
N3 C9 H9E 108.2 . . ?
C10 C9 H9D 108.2 . . ?
C10 C9 H9E 108.2 . . ?
H9D C9 H9E 107.4 . . ?
C12 C11 H11D 109.1 . . ?
C12 C11 H11E 109.1 . . ?
C10 C11 C12 112.7(11) . . ?
C10 C11 H11D 109.1 . . ?
C10 C11 H11E 109.1 . . ?
H11D C11 H11E 107.8 . . ?
C16 C15 H15A 109.0 . . ?
C16 C15 H15B 109.0 . . ?
C16 C15 C14 112.9(12) . . ?
H15A C15 H15B 107.8 . . ?
C14 C15 H15A 109.0 . . ?
C14 C15 H15B 109.0 . . ?
C18 C19 C20 113.8(10) . . ?
C18 C19 H19A 108.8 . . ?
C18 C19 H19B 108.8 . . ?
C20 C19 H19A 108.8 . . ?
C20 C19 H19B 108.8 . . ?
H19A C19 H19B 107.7 . . ?
C41 C42 H42A 108.5 . . ?
C41 C42 H42B 108.5 . . ?
C41 C42 C43 114.9(12) . . ?
H42A C42 H42B 107.5 . . ?
C43 C42 H42A 108.5 . . ?
C43 C42 H42B 108.5 . . ?
C40 C39 H39A 108.3 . . ?
C40 C39 H39B 108.3 . . ?
C40 C39 C38 116.0(11) . . ?
H39A C39 H39B 107.4 . . ?
C38 C39 H39A 108.3 . . ?
C38 C39 H39B 108.3 . . ?
C37 C38 C39 116.2(12) . . ?
C37 C38 H38A 108.2 . . ?
C37 C38 H38B 108.2 . . ?
C39 C38 H38A 108.2 . . ?
C39 C38 H38B 108.2 . . ?
H38A C38 H38B 107.4 . . ?
C44 C43 H43A 108.3 . . ?
C44 C43 H43B 108.3 . . ?
C42 C43 C44 116.1(11) . . ?
C42 C43 H43A 108.3 . . ?
C42 C43 H43B 108.3 . . ?
H43A C43 H43B 107.4 . . ?
C24 C23 H23A 108.7 . . ?
C24 C23 H23B 108.7 . . ?
C22 C23 C24 114.3(12) . . ?
C22 C23 H23A 108.7 . . ?
C22 C23 H23B 108.7 . . ?
H23A C23 H23B 107.6 . . ?
C15 C14 H14A 107.3 . . ?
C15 C14 H14B 107.3 . . ?
H14A C14 H14B 106.9 . . ?
C13 C14 C15 120.2(13) . . ?
C13 C14 H14A 107.3 . . ?
C13 C14 H14B 107.3 . . ?
N4 C13 H13A 108.2 . . ?
N4 C13 H13B 108.2 . . ?
C14 C13 N4 116.4(12) . . ?
C14 C13 H13A 108.2 . . ?
C14 C13 H13B 108.2 . . ?
H13A C13 H13B 107.3 . . ?

_olex2_submission_original_sample_id AJ80
_olex2_submission_special_instructions 'No special instructions were received'
