# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1417496'
_audit_update_record             
;
2015-10-13 deposited with the CCDC.
2015-10-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Br4 Pb, 2(C2 H6 N), 4(C H3)'
_chemical_formula_sum            'C8 H24 Br4 N2 Pb'
_chemical_formula_weight         675.09

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

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                   14.196(3)
_cell_length_b                   8.3416(17)
_cell_length_c                   8.2422(16)
_cell_angle_alpha                90
_cell_angle_beta                 105.32(3)
_cell_angle_gamma                90
_cell_volume                     941.3(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    0
_cell_measurement_theta_min      -1.#IN
_cell_measurement_theta_max      -1.#IN

_exptl_crystal_description       plate
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.382
_exptl_crystal_F_000             616.0
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_absorpt_coefficient_mu    17.433
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.021
_exptl_absorpt_correction_T_max  0.031
_exptl_absorpt_process_details   'CrystalClear (Rigaku, 2005)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Rigaku Mercury CCD'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6231
_diffrn_reflns_av_unetI/netI     0.1375
_diffrn_reflns_av_R_equivalents  0.1100
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.540
_diffrn_reflns_theta_max         27.477
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             2155
_reflns_number_gt                1300
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0423P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2155
_refine_ls_number_parameters     115
_refine_ls_number_restraints     103
_refine_ls_R_factor_all          0.1144
_refine_ls_R_factor_gt           0.0668
_refine_ls_wR_factor_ref         0.1431
_refine_ls_wR_factor_gt          0.1288
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_restrained_S_all      0.990
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000

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
C1 C 0.4051(14) 1.1299(14) 0.683(3) 0.130(5) Uani 0.458(11) 1 d D U P A 1
H1A H 0.3684 1.2116 0.6112 0.195 Uiso 0.458(11) 1 calc R U P A 1
H1B H 0.4567 1.0929 0.6367 0.195 Uiso 0.458(11) 1 calc R U P A 1
H1C H 0.4326 1.1731 0.7930 0.195 Uiso 0.458(11) 1 calc R U P A 1
C3 C 0.3431(8) 1.0010(16) 0.6931(15) 0.127(3) Uani 0.5 1 d D U P A 1
H3 H 0.3364 1.0382 0.8022 0.152 Uiso 0.5 1 calc R U P A 1
C2' C 0.3961(15) 0.8458(12) 0.773(2) 0.147(5) Uani 0.542(11) 1 d D U P A 1
H2'1 H 0.4587 0.8730 0.8464 0.221 Uiso 0.542(11) 1 calc R U P A 1
H2'2 H 0.4049 0.7756 0.6860 0.221 Uiso 0.542(11) 1 calc R U P A 1
H2'3 H 0.3575 0.7928 0.8367 0.221 Uiso 0.542(11) 1 calc R U P A 1
H4A H 0.1895(19) 0.876(3) 0.61(4) 0.221 Uiso 0.458(11) 1 d D U P A 1
H4B H 0.2240(17) 1.029(2) 0.7262(14) 0.221 Uiso 0.458(11) 1 d D U P A 1
C1' C 0.3974(13) 1.019(2) 0.5652(14) 0.131(5) Uani 0.542(11) 1 d D U P A 2
H1'1 H 0.3771 0.9512 0.4678 0.197 Uiso 0.542(11) 1 calc R U P A 2
H1'2 H 0.4654 1.0009 0.6182 0.197 Uiso 0.542(11) 1 calc R U P A 2
H1'3 H 0.3874 1.1289 0.5319 0.197 Uiso 0.542(11) 1 calc R U P A 2
C3' C 0.3451(9) 0.9837(15) 0.6731(17) 0.127(3) Uani 0.5 1 d D U P A 2
H3' H 0.3430 1.0957 0.7079 0.152 Uiso 0.5 1 calc R U P A 2
C2 C 0.3970(17) 0.927(3) 0.8534(13) 0.140(5) Uani 0.458(11) 1 d D U P A 2
H2A H 0.3838 0.8156 0.8649 0.210 Uiso 0.458(11) 1 calc R U P A 2
H2B H 0.3734 0.9883 0.9333 0.210 Uiso 0.458(11) 1 calc R U P A 2
H2C H 0.4662 0.9431 0.8740 0.210 Uiso 0.458(11) 1 calc R U P A 2
H4A' H 0.1888(18) 0.877(3) 0.61(3) 0.210 Uiso 0.542(11) 1 d D U P A 2
H4B' H 0.2239(17) 1.029(2) 0.7262(14) 0.210 Uiso 0.542(11) 1 d D U P A 2
C4 C 0.2368(6) 0.9650(10) 0.6341(11) 0.113(3) Uani 1 1 d D U . . .
N1 N 0.1828(5) 1.0753(9) 0.5089(7) 0.077(2) Uani 1 1 d D U . . .
H1D H 0.1213 1.0808 0.5154 0.116 Uiso 1 1 calc DR U . . .
H1E H 0.1838 1.0412 0.4070 0.116 Uiso 1 1 calc R U . . .
H1F H 0.2101 1.1720 0.5270 0.116 Uiso 1 1 calc DR U . . .
Pb1 Pb 0.0000 0.0000 0.0000 0.04325(13) Uani 1 2 d S . P . .
Br1 Br -0.00334(7) 0.30908(10) 0.18882(8) 0.0567(3) Uani 1 1 d . . . . .
Br2 Br 0.21756(8) 0.02655(12) 0.11441(11) 0.0703(3) Uani 1 1 d . . . . .


_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
C1 C3 1.406(19) . ?
C3 C4 1.489(12) . ?
C3 C2' 1.554(14) . ?
C1' C3' 1.33(2) . ?
C3' C4 1.494(13) . ?
C3' C2 1.547(14) . ?
C4 N1 1.442(9) . ?
Pb1 Br2 2.9895(14) 3 ?
Pb1 Br2 2.9895(14) . ?
Pb1 Br1 3.0088(8) 4_565 ?
Pb1 Br1 3.0088(8) 2_545 ?
Pb1 Br1 3.0183(9) 3 ?
Pb1 Br1 3.0183(9) . ?
Br1 Pb1 3.0087(8) 2 ?

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
C1 C3 C4 137.0(12) . . ?
C1 C3 C2' 115.0(12) . . ?
C4 C3 C2' 107.8(12) . . ?
C1' C3' C4 127.0(11) . . ?
C1' C3' C2 120.0(13) . . ?
C4 C3' C2 112.1(13) . . ?
N1 C4 C3 113.9(8) . . ?
N1 C4 C3' 114.1(8) . . ?
Br2 Pb1 Br2 180.0 3 . ?
Br2 Pb1 Br1 89.32(4) 3 4_565 ?
Br2 Pb1 Br1 90.68(4) . 4_565 ?
Br2 Pb1 Br1 90.68(4) 3 2_545 ?
Br2 Pb1 Br1 89.32(4) . 2_545 ?
Br1 Pb1 Br1 180.00(4) 4_565 2_545 ?
Br2 Pb1 Br1 85.97(3) 3 3 ?
Br2 Pb1 Br1 94.03(3) . 3 ?
Br1 Pb1 Br1 90.657(16) 4_565 3 ?
Br1 Pb1 Br1 89.343(16) 2_545 3 ?
Br2 Pb1 Br1 94.03(3) 3 . ?
Br2 Pb1 Br1 85.97(3) . . ?
Br1 Pb1 Br1 89.343(16) 4_565 . ?
Br1 Pb1 Br1 90.657(16) 2_545 . ?
Br1 Pb1 Br1 180.0 3 . ?
Pb1 Br1 Pb1 153.23(3) 2 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C3 C4 N1 14(2) . . . . ?
C2' C3 C4 N1 -159.9(11) . . . . ?
C1' C3' C4 N1 -37.3(19) . . . . ?
C2 C3' C4 N1 153.3(11) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1F Br2 0.89 2.61 3.435(7) 154.7 4_576
N1 H1E Br2 0.89 2.58 3.439(6) 161.6 1_565
N1 H1D Br1 0.89 3.05 3.448(7) 109.5 2
N1 H1D Br1 0.89 2.71 3.491(7) 146.7 4_576

_refine_diff_density_max         2.477
_refine_diff_density_min         -3.812
_refine_diff_density_rms         0.304

####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1417497'
_audit_update_record             
;
2015-10-13 deposited with the CCDC.
2015-10-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Br4 Pb, 2(C4 H12 N)'
_chemical_formula_sum            'C8 H24 Br4 N2 Pb'
_chemical_formula_weight         675.09

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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           64
_space_group_name_H-M_alt        'C m c a'
_space_group_name_Hall           '-C 2bc 2'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y+1/2, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y-1/2, -z-1/2'
'x, -y-1/2, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y, -z-1/2'
'x+1/2, -y, z-1/2'
'-x+1/2, y+1/2, z'

_cell_length_a                   28.12(3)
_cell_length_b                   8.312(8)
_cell_length_c                   8.309(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1942(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    393(2)
_cell_measurement_reflns_used    1997
_cell_measurement_theta_min      2.8477
_cell_measurement_theta_max      27.3277

_exptl_crystal_description       plate
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.309
_exptl_crystal_F_000             1232.0
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_absorpt_coefficient_mu    16.899
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.024
_exptl_absorpt_correction_T_max  0.034
_exptl_absorpt_process_details   'CrystalClear (Rigaku, 2005)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      393(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Rigaku Mercury CCD'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9718
_diffrn_reflns_av_unetI/netI     0.0667
_diffrn_reflns_av_R_equivalents  0.1345
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.898
_diffrn_reflns_theta_max         27.473
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1135
_reflns_number_gt                838
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0522P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1135
_refine_ls_number_parameters     58
_refine_ls_number_restraints     31
_refine_ls_R_factor_all          0.0862
_refine_ls_R_factor_gt           0.0588
_refine_ls_wR_factor_ref         0.1354
_refine_ls_wR_factor_gt          0.1209
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_restrained_S_all      1.110
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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 0.0624(3) Uani 1 4 d S T P . .
Br1 Br 0.5000 0.30964(16) 0.69033(16) 0.0837(6) Uani 1 2 d S T P . .
Br2 Br 0.39391(11) 0.0000 0.5000 0.1161(8) Uani 1 2 d S T P . .
C4 C 0.3782(10) 0.0000 1.0000 0.183(14) Uani 1 2 d DS TU P . .
H4A H 0.3802 0.0452 1.1061 0.219 Uiso 0.5 1 d R U P . .
H4B H 0.3910 -0.1067 1.0087 0.219 Uiso 0.5 1 d R U P . .
N1 N 0.4126(9) 0.080(3) 0.916(3) 0.128(8) Uani 0.5 1 d D U P . .
H1D H 0.4412 0.0723 0.9642 0.192 Uiso 0.5 1 d R U P . .
H1E H 0.4144 0.0383 0.8161 0.192 Uiso 0.5 1 d R U P . .
H1F H 0.4040 0.1841 0.9096 0.192 Uiso 0.5 1 d R U P . .
C3 C 0.3262(12) -0.022(5) 0.978(6) 0.224(15) Uani 0.5 1 d D U P . .
H3A H 0.3164 -0.1194 0.9253 0.269 Uiso 0.5 1 d R U P . .
C1 C 0.3121(15) 0.146(6) 0.926(9) 0.26(2) Uani 0.5 1 d D U P . .
H1A H 0.3221 0.1447 0.8151 0.387 Uiso 0.5 1 d R U P . .
H1B H 0.2783 0.1604 0.9308 0.387 Uiso 0.5 1 d R U P . .
H1C H 0.3277 0.2322 0.9812 0.387 Uiso 0.5 1 d R U P . .
C2 C 0.3098(15) -0.015(8) 1.150(7) 0.27(2) Uani 0.5 1 d D U P . .
H2A H 0.3156 -0.1068 1.2171 0.407 Uiso 0.5 1 d R U P . .
H2B H 0.3256 0.0775 1.1955 0.407 Uiso 0.5 1 d R U P . .
H2C H 0.2762 0.0057 1.1451 0.407 Uiso 0.5 1 d R U P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br2 2.983(4) 9_656 ?
Pb1 Br2 2.983(4) . ?
Pb1 Br1 3.021(2) 2_654 ?
Pb1 Br1 3.021(2) 10_557 ?
Pb1 Br1 3.021(3) . ?
Pb1 Br1 3.021(3) 9_656 ?
Br1 Pb1 3.021(2) 2_655 ?
C4 N1 1.366(16) 4_557 ?
C4 N1 1.366(16) . ?
C4 C3 1.49(2) 4_557 ?
C4 C3 1.49(2) . ?
C3 C3 0.52(9) 4_557 ?
C3 C2 1.20(8) 4_557 ?
C3 C1 1.36(7) 4_557 ?
C3 C2 1.50(2) . ?
C3 C1 1.51(2) . ?
C1 C2 1.26(8) 4_557 ?
C1 C3 1.36(6) 4_557 ?
C2 C3 1.20(8) 4_557 ?
C2 C1 1.26(8) 4_557 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br2 Pb1 Br2 180.0 9_656 . ?
Br2 Pb1 Br1 90.0 9_656 2_654 ?
Br2 Pb1 Br1 90.0 . 2_654 ?
Br2 Pb1 Br1 90.0 9_656 10_557 ?
Br2 Pb1 Br1 90.0 . 10_557 ?
Br1 Pb1 Br1 180.0 2_654 10_557 ?
Br2 Pb1 Br1 90.0 9_656 . ?
Br2 Pb1 Br1 90.0 . . ?
Br1 Pb1 Br1 89.97(7) 2_654 . ?
Br1 Pb1 Br1 90.03(7) 10_557 . ?
Br2 Pb1 Br1 90.0 9_656 9_656 ?
Br2 Pb1 Br1 90.0 . 9_656 ?
Br1 Pb1 Br1 90.03(7) 2_654 9_656 ?
Br1 Pb1 Br1 89.97(7) 10_557 9_656 ?
Br1 Pb1 Br1 180.0 . 9_656 ?
Pb1 Br1 Pb1 153.16(6) 2_655 . ?
N1 C4 N1 90(3) 4_557 . ?
N1 C4 C3 134(2) 4_557 4_557 ?
N1 C4 C3 134(2) . 4_557 ?
N1 C4 C3 134(2) 4_557 . ?
N1 C4 C3 134(2) . . ?
C3 C4 C3 20(4) 4_557 . ?
C3 C3 C2 116(8) 4_557 4_557 ?
C3 C3 C1 97(10) 4_557 4_557 ?
C2 C3 C1 127(4) 4_557 4_557 ?
C3 C3 C4 80.0(18) 4_557 . ?
C2 C3 C4 117(5) 4_557 . ?
C1 C3 C4 108(3) 4_557 . ?
C3 C3 C2 46(7) 4_557 . ?
C2 C3 C2 136(6) 4_557 . ?
C1 C3 C2 52(4) 4_557 . ?
C4 C3 C2 100.4(17) . . ?
C3 C3 C1 63(8) 4_557 . ?
C2 C3 C1 54(4) 4_557 . ?
C1 C3 C1 142(4) 4_557 . ?
C4 C3 C1 100.2(17) . . ?
C2 C3 C1 99.0(17) . . ?
C2 C1 C3 70(3) 4_557 4_557 ?
C2 C1 C3 50(3) 4_557 . ?
C3 C1 C3 20(4) 4_557 . ?
C3 C2 C1 76(5) 4_557 4_557 ?
C3 C2 C3 18(4) 4_557 . ?
C1 C2 C3 58(4) 4_557 . ?

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 C4 C3 C3 99(9) 4_557 . . 4_557 ?
N1 C4 C3 C3 -101(10) . . . 4_557 ?
N1 C4 C3 C2 -147(4) 4_557 . . 4_557 ?
N1 C4 C3 C2 14(7) . . . 4_557 ?
C3 C4 C3 C2 114(10) 4_557 . . 4_557 ?
N1 C4 C3 C1 5(6) 4_557 . . 4_557 ?
N1 C4 C3 C1 165(4) . . . 4_557 ?
C3 C4 C3 C1 -94(11) 4_557 . . 4_557 ?
N1 C4 C3 C2 58(4) 4_557 . . . ?
N1 C4 C3 C2 -142(3) . . . . ?
C3 C4 C3 C2 -41(8) 4_557 . . . ?
N1 C4 C3 C1 159(3) 4_557 . . . ?
N1 C4 C3 C1 -41(4) . . . . ?
C3 C4 C3 C1 60(8) 4_557 . . . ?
C3 C3 C1 C2 -171(7) 4_557 . . 4_557 ?
C1 C3 C1 C2 -106(4) 4_557 . . 4_557 ?
C4 C3 C1 C2 116(6) . . . 4_557 ?
C2 C3 C1 C2 -142(7) . . . 4_557 ?
C2 C3 C1 C3 171(7) 4_557 . . 4_557 ?
C1 C3 C1 C3 65(9) 4_557 . . 4_557 ?
C4 C3 C1 C3 -73(3) . . . 4_557 ?
C2 C3 C1 C3 29(3) . . . 4_557 ?
C2 C3 C2 C3 -83(9) 4_557 . . 4_557 ?
C1 C3 C2 C3 170(9) 4_557 . . 4_557 ?
C4 C3 C2 C3 65(6) . . . 4_557 ?
C1 C3 C2 C3 -37(6) . . . 4_557 ?
C3 C3 C2 C1 -170(9) 4_557 . . 4_557 ?
C2 C3 C2 C1 107(5) 4_557 . . 4_557 ?
C4 C3 C2 C1 -105(4) . . . 4_557 ?
C1 C3 C2 C1 153(5) . . . 4_557 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1F Br2 0.90 2.75 3.60(2) 158.7 10_567
N1 H1E Br2 0.90 2.71 3.56(2) 157.9 .
N1 H1D Br1 0.90 3.03 3.44(3) 110.5 10_557
N1 H1D Br1 0.90 2.69 3.48(3) 146.6 2_655

_refine_diff_density_max         1.280
_refine_diff_density_min         -0.913
_refine_diff_density_rms         0.207

