# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_8_T320K_17CGC005
_database_code_depnum_ccdc_archive 'CCDC 1855518'
loop_
_audit_author_name
_audit_author_address
'Antonio L. Llamas-Saiz'
;Universidade de Santiago de Compostela
Spain
;
_audit_update_record             
;
2018-07-13 deposited with the CCDC.	2019-07-23 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            'DMAPbCl3D - T320K'
_chemical_formula_moiety         'Cl3 Pb'
_chemical_formula_sum            'Cl3 Pb'
_chemical_formula_iupac          ?
_chemical_formula_weight         313.54

_chemical_melting_point          ?

_space_group_crystal_system      hexagonal
_space_group_name_H-M_alt        'P 63/m m c'
_space_group_name_Hall           '-P 6c 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, z-1/2'

_cell_length_a                   8.3732(3)
_cell_length_b                   8.3732(3)
_cell_length_c                   13.9808(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     848.88(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2830
_cell_measurement_theta_min      2.8090
_cell_measurement_theta_max      20.8441
_cell_measurement_temperature    320.(2)

_exptl_crystal_description       plate
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_size_max          0.278
_exptl_crystal_size_mid          0.168
_exptl_crystal_size_min          0.038
_exptl_crystal_density_diffrn    2.453
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             532

_exptl_absorpt_coefficient_mu    20.702
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
'TWINABS - Bruker AXS scaling for twinned crystals - Version 2012/1'
_exptl_absorpt_correction_T_min  0.10
_exptl_absorpt_correction_T_max  0.51

_exptl_special_details           
;
;

_diffrn_ambient_temperature      320.(2)

_diffrn_source                   'sealed x-ray tube'
_diffrn_source_type              'SIEMENS KFN MO 2K-90'

_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device       'κ--geometry diffractometer'
_diffrn_measurement_device_type  'Bruker AXS X8 APEX-II'
_diffrn_measurement_method       'φ or ω oscillation scans'

_diffrn_detector_area_resol_mean 16.6666

_diffrn_reflns_number            806
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_unetI/netI     0.0228
_diffrn_reflns_theta_min         2.81
_diffrn_reflns_theta_max         23.85
_diffrn_reflns_theta_full        23.85
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       15

_refine_special_details          'Refined as a 2-component twin.,Twin,SQUEEZE'

_reflns_number_total             806
_reflns_number_gt                655
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0517
_refine_ls_wR_factor_gt          0.1458
_refine_ls_wR_factor_ref         0.1580
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_restrained_S_all      1.097
_refine_ls_number_reflns         806
_refine_ls_number_parameters     13
_refine_ls_number_restraints     0
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    undef
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0877P)²+5.0882P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap

_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.467
_refine_diff_density_min         -0.670
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cl Cl 0.1484 0.1585 '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'

_computing_data_collection       'Bruker APEX3 software'
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 833)'
_computing_publication_material  ?

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb Pb01 0.333333 0.666667 0.38858(11) 0.0756(8) Uani d T P S 1 . .
Cl Cl02 0.1893(7) 0.8107(7) 0.25 0.150(5) Uani d T P S 1 . .
Cl Cl03 0.5 1.0 0.5 0.208(8) Uani d T P S 1 . .


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pb01 Cl02 2_665 2.849(8) ?
Pb01 Cl02 3_565 2.849(7) ?
Pb01 Cl02 . 2.849(7) ?
Pb01 Cl03 . 2.8756(9) ?
Pb01 Cl03 2_665 2.8756(9) ?
Pb01 Cl03 3_565 2.8756(9) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl02 Pb01 Cl02 2_665 3_565 78.8(2) ?
Cl02 Pb01 Cl02 2_665 . 78.8(2) ?
Cl02 Pb01 Cl02 3_565 . 78.8(2) ?
Cl02 Pb01 Cl03 2_665 . 169.96(15) ?
Cl02 Pb01 Cl03 3_565 . 93.45(10) ?
Cl02 Pb01 Cl03 . . 93.45(10) ?
Cl02 Pb01 Cl03 2_665 2_665 93.45(10) ?
Cl02 Pb01 Cl03 3_565 2_665 169.96(15) ?
Cl02 Pb01 Cl03 . 2_665 93.45(10) ?
Cl03 Pb01 Cl03 . 2_665 93.43(4) ?
Cl02 Pb01 Cl03 2_665 3_565 93.45(9) ?
Cl02 Pb01 Cl03 3_565 3_565 93.45(9) ?
Cl02 Pb01 Cl03 . 3_565 169.96(15) ?
Cl03 Pb01 Cl03 . 3_565 93.43(4) ?
Cl03 Pb01 Cl03 2_665 3_565 93.43(4) ?
Pb01 Cl02 Pb01 16_556 . 85.7(3) ?
Pb01 Cl03 Pb01 . 13_676 180.0 ?

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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Cl02 Pb01 Cl02 Pb01 2_665 . . 16_556 -40.33(8) ?
Cl02 Pb01 Cl02 Pb01 3_565 . . 16_556 40.33(7) ?
Cl03 Pb01 Cl02 Pb01 . . . 16_556 133.175(19) ?
Cl03 Pb01 Cl02 Pb01 2_665 . . 16_556 -133.175(19) ?
Cl03 Pb01 Cl02 Pb01 3_565 . . 16_556 0.000(2) ?



_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: DMF'
####################################################################### 
# 
# 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_4_T100K_17CGC005
_database_code_depnum_ccdc_archive 'CCDC 1855519'
loop_
_audit_author_name
_audit_author_address
'Antonio L. Llamas-Saiz'
;Universidade de Santiago de Compostela
Spain
;
_audit_update_record             
;
2018-07-12 deposited with the CCDC.	2019-07-23 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            'DMAPbCl3D - T100K'
_chemical_formula_moiety         'Cl6 Pb2, 2(C2 H8 N)'
_chemical_formula_sum            'C4 H16 Cl6 N2 Pb2'
_chemical_formula_iupac          ?
_chemical_formula_weight         719.27
_chemical_absolute_configuration ad

_chemical_melting_point          ?

_space_group_crystal_system      orthorhombic
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x+1/2, -y, z+1/2'

_cell_length_a                   8.5000(2)
_cell_length_b                   13.4458(4)
_cell_length_c                   14.1302(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1614.93(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9265
_cell_measurement_theta_min      2.7965
_cell_measurement_theta_max      31.6238
_cell_measurement_temperature    100.(2)

_exptl_crystal_description       plate
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.030
_exptl_crystal_density_diffrn    2.958
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1280

_exptl_absorpt_coefficient_mu    21.787
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
'TWINABS - Bruker AXS scaling for twinned crystals - Version 2012/1'
_exptl_absorpt_correction_T_min  0.0304
_exptl_absorpt_correction_T_max  0.1259

_exptl_special_details           
;
;

_diffrn_ambient_temperature      100.(2)

_diffrn_source                   'sealed x-ray tube'
_diffrn_source_type              'SIEMENS KFN MO 2K-90'

_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device       'κ--geometry diffractometer'
_diffrn_measurement_device_type  'Bruker AXS X8 APEX-II'
_diffrn_measurement_method       'φ or ω oscillation scans'

_diffrn_detector_area_resol_mean 16.6666

_diffrn_reflns_number            14329
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0526
_diffrn_reflns_theta_min         2.09
_diffrn_reflns_theta_max         33.31
_diffrn_reflns_theta_full        33.31
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21

_refine_special_details          'Refined as a 4-component twin.,Twin'

_reflns_number_total             14329
_reflns_number_gt                12854
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0426
_refine_ls_wR_factor_gt          0.1097
_refine_ls_wR_factor_ref         0.1142
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_refine_ls_number_reflns         14329
_refine_ls_number_parameters     134
_refine_ls_number_restraints     0
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0824P)²] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap

_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         2.795
_refine_diff_density_min         -4.597
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
;

Flack x determined using 2395 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.001(5)

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'
Cl Cl 0.1484 0.1585 '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'

_computing_data_collection       'Bruker APEX3 software'
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 882)'
_computing_publication_material  ?

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb Pb1 0.28942(5) 0.31381(3) 0.37876(3) 0.01405(10) Uani d . . . 1 . .
Pb Pb2 0.31180(5) 0.33753(3) 0.10493(3) 0.01418(10) Uani d . . . 1 . .
Cl Cl1 0.0285(4) 0.2188(2) 0.4795(2) 0.0201(6) Uani d . . . 1 . .
Cl Cl2 0.2732(4) 0.4938(2) 0.4604(2) 0.0203(6) Uani d . . . 1 . .
Cl Cl3 0.1008(4) 0.4102(2) 0.2405(2) 0.0188(5) Uani d . . . 1 . .
Cl Cl4 0.5293(4) 0.3898(2) 0.2608(2) 0.0206(6) Uani d . . . 1 . .
Cl Cl5 0.3056(4) 0.16659(19) 0.2046(2) 0.0190(5) Uani d . . . 1 . .
Cl Cl6 0.0797(4) 0.2540(3) -0.0119(3) 0.0273(7) Uani d . . . 1 . .
N N11 0.2939(13) 0.6413(8) 0.2790(8) 0.022(2) Uani d . . . 1 . .
H H11A 0.285587 0.580801 0.307512 0.027 Uiso calc U . R 1 . .
H H11B 0.373287 0.675076 0.30783 0.027 Uiso calc U . R 1 . .
C C12 0.1452(17) 0.6965(12) 0.2924(11) 0.030(3) Uani d . . . 1 . .
H H12A 0.122741 0.702589 0.360147 0.045 Uiso calc U . R 1 . .
H H12B 0.059153 0.660575 0.261327 0.045 Uiso calc U . R 1 . .
H H12C 0.155075 0.762937 0.264486 0.045 Uiso calc U . R 1 . .
C C13 0.3342(16) 0.6267(10) 0.1781(9) 0.022(2) Uani d . . . 1 . .
H H13A 0.240576 0.604582 0.143447 0.033 Uiso calc U . R 1 . .
H H13B 0.416857 0.57618 0.172632 0.033 Uiso calc U . R 1 . .
H H13C 0.371791 0.68954 0.151271 0.033 Uiso calc U . R 1 . .
N N21 0.6827(13) 0.4993(8) 0.4658(8) 0.023(2) Uani d . . . 1 . .
H H21A 0.612578 0.448855 0.457681 0.028 Uiso calc U . R 1 . .
H H21B 0.646902 0.55258 0.432452 0.028 Uiso calc U . R 1 . .
C C22 0.687(2) 0.5261(11) 0.5679(11) 0.033(3) Uani d . . . 1 . .
H H22A 0.770531 0.575262 0.578657 0.049 Uiso calc U . R 1 . .
H H22B 0.708835 0.466423 0.605552 0.049 Uiso calc U . R 1 . .
H H22C 0.585697 0.554251 0.586699 0.049 Uiso calc U . R 1 . .
C C23 0.8361(17) 0.4684(10) 0.4262(11) 0.028(3) Uani d . . . 1 . .
H H23A 0.916288 0.517849 0.442575 0.042 Uiso calc U . R 1 . .
H H23B 0.827852 0.463096 0.357239 0.042 Uiso calc U . R 1 . .
H H23C 0.865892 0.403662 0.452658 0.042 Uiso calc U . R 1 . .


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pb1 Cl2 . 2.685(3) ?
Pb1 Cl4 . 2.825(3) ?
Pb1 Cl3 . 2.840(3) ?
Pb1 Cl1 2_556 2.887(3) ?
Pb1 Cl1 . 2.928(3) ?
Pb2 Cl5 . 2.696(3) ?
Pb2 Cl3 . 2.800(3) ?
Pb2 Cl6 . 2.807(3) ?
Pb2 Cl6 2 2.903(3) ?
Pb2 Cl4 . 2.961(3) ?
N11 C12 . 1.478(17) ?
N11 C13 . 1.480(17) ?
N11 H11A . 0.91 ?
N11 H11B . 0.91 ?
C12 H12A . 0.98 ?
C12 H12B . 0.98 ?
C12 H12C . 0.98 ?
C13 H13A . 0.98 ?
C13 H13B . 0.98 ?
C13 H13C . 0.98 ?
N21 C23 . 1.479(17) ?
N21 C22 . 1.487(19) ?
N21 H21A . 0.91 ?
N21 H21B . 0.91 ?
C22 H22A . 0.98 ?
C22 H22B . 0.98 ?
C22 H22C . 0.98 ?
C23 H23A . 0.98 ?
C23 H23B . 0.98 ?
C23 H23C . 0.98 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl2 Pb1 Cl4 . . 87.97(10) ?
Cl2 Pb1 Cl3 . . 81.68(9) ?
Cl4 Pb1 Cl3 . . 80.60(10) ?
Cl2 Pb1 Cl1 . 2_556 82.81(9) ?
Cl4 Pb1 Cl1 . 2_556 87.47(10) ?
Cl3 Pb1 Cl1 . 2_556 160.71(9) ?
Cl2 Pb1 Cl1 . . 98.37(9) ?
Cl4 Pb1 Cl1 . . 172.39(9) ?
Cl3 Pb1 Cl1 . . 96.08(9) ?
Cl1 Pb1 Cl1 2_556 . 97.45(2) ?
Cl5 Pb2 Cl3 . . 85.84(9) ?
Cl5 Pb2 Cl6 . . 87.28(10) ?
Cl3 Pb2 Cl6 . . 95.28(11) ?
Cl5 Pb2 Cl6 . 2 83.71(10) ?
Cl3 Pb2 Cl6 . 2 163.74(10) ?
Cl6 Pb2 Cl6 . 2 96.628(17) ?
Cl5 Pb2 Cl4 . . 79.97(9) ?
Cl3 Pb2 Cl4 . . 78.93(9) ?
Cl6 Pb2 Cl4 . . 166.31(9) ?
Cl6 Pb2 Cl4 2 . 86.99(10) ?
Pb1 Cl1 Pb1 2_456 . 159.46(12) ?
Pb2 Cl3 Pb1 . . 87.13(8) ?
Pb1 Cl4 Pb2 . . 84.38(8) ?
Pb2 Cl6 Pb2 . 2_455 170.82(15) ?
C12 N11 C13 . . 112.8(11) ?
C12 N11 H11A . . 109.0 ?
C13 N11 H11A . . 109.0 ?
C12 N11 H11B . . 109.0 ?
C13 N11 H11B . . 109.0 ?
H11A N11 H11B . . 107.8 ?
N11 C12 H12A . . 109.5 ?
N11 C12 H12B . . 109.5 ?
H12A C12 H12B . . 109.5 ?
N11 C12 H12C . . 109.5 ?
H12A C12 H12C . . 109.5 ?
H12B C12 H12C . . 109.5 ?
N11 C13 H13A . . 109.5 ?
N11 C13 H13B . . 109.5 ?
H13A C13 H13B . . 109.5 ?
N11 C13 H13C . . 109.5 ?
H13A C13 H13C . . 109.5 ?
H13B C13 H13C . . 109.5 ?
C23 N21 C22 . . 114.3(12) ?
C23 N21 H21A . . 108.7 ?
C22 N21 H21A . . 108.7 ?
C23 N21 H21B . . 108.7 ?
C22 N21 H21B . . 108.7 ?
H21A N21 H21B . . 107.6 ?
N21 C22 H22A . . 109.5 ?
N21 C22 H22B . . 109.5 ?
H22A C22 H22B . . 109.5 ?
N21 C22 H22C . . 109.5 ?
H22A C22 H22C . . 109.5 ?
H22B C22 H22C . . 109.5 ?
N21 C23 H23A . . 109.5 ?
N21 C23 H23B . . 109.5 ?
H23A C23 H23B . . 109.5 ?
N21 C23 H23C . . 109.5 ?
H23A C23 H23C . . 109.5 ?
H23B C23 H23C . . 109.5 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Cl2 Pb1 Cl1 Pb1 . . . 2_456 -15.8(4) ?
Cl4 Pb1 Cl1 Pb1 . . . 2_456 -161.9(6) ?
Cl3 Pb1 Cl1 Pb1 . . . 2_456 -98.2(4) ?
Cl1 Pb1 Cl1 Pb1 2_556 . . 2_456 68.0(4) ?
Cl5 Pb2 Cl3 Pb1 . . . . 41.94(8) ?
Cl6 Pb2 Cl3 Pb1 . . . . 128.82(10) ?
Cl6 Pb2 Cl3 Pb1 2 . . . -8.1(4) ?
Cl4 Pb2 Cl3 Pb1 . . . . -38.64(8) ?
Cl2 Pb1 Cl3 Pb2 . . . . 129.93(10) ?
Cl4 Pb1 Cl3 Pb2 . . . . 40.62(9) ?
Cl1 Pb1 Cl3 Pb2 2_556 . . . 93.2(3) ?
Cl1 Pb1 Cl3 Pb2 . . . . -132.46(9) ?
Cl2 Pb1 Cl4 Pb2 . . . . -120.07(9) ?
Cl3 Pb1 Cl4 Pb2 . . . . -38.17(8) ?
Cl1 Pb1 Cl4 Pb2 2_556 . . . 157.05(8) ?
Cl1 Pb1 Cl4 Pb2 . . . . 26.5(8) ?
Cl5 Pb2 Cl4 Pb1 . . . . -48.63(9) ?
Cl3 Pb2 Cl4 Pb1 . . . . 39.05(8) ?
Cl6 Pb2 Cl4 Pb1 . . . . -26.9(5) ?
Cl6 Pb2 Cl4 Pb1 2 . . . -132.76(10) ?
Cl5 Pb2 Cl6 Pb2 . . . 2_455 54.1(10) ?
Cl3 Pb2 Cl6 Pb2 . . . 2_455 -31.4(10) ?
Cl6 Pb2 Cl6 Pb2 2 . . 2_455 137.5(11) ?
Cl4 Pb2 Cl6 Pb2 . . . 2_455 32.8(13) ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N11 H11A Cl2 . 0.91 2.46 3.246(11) 144.8 ?
N11 H11A Cl3 . 0.91 2.94 3.556(12) 126.6 ?
N11 H11A Cl4 . 0.91 3.36 3.937(12) 123.2 ?
N11 H11B Cl4 3_655 0.91 3.16 3.707(12) 120.9 ?
N11 H11B Cl5 3_655 0.91 2.74 3.429(12) 133.6 ?
N11 H11B Cl6 4_565 0.91 2.75 3.444(11) 134.1 ?
N21 H21A Cl1 2_556 0.91 2.53 3.303(11) 143.7 ?
N21 H21A Cl2 . 0.91 2.95 3.483(12) 119.1 ?
N21 H21A Cl4 . 0.91 2.98 3.501(12) 118.2 ?
N21 H21B Cl5 3_655 0.91 2.50 3.297(12) 146.0 ?
N21 H21B Cl6 4_565 0.91 3.33 4.010(12) 133.3 ?


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: DMF'
####################################################################### 
# 
# 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_6_T100K_2016cg06
_database_code_depnum_ccdc_archive 'CCDC 1855520'
loop_
_audit_author_name
_audit_author_address
'Antonio L. Llamas-Saiz'
;Universidade de Santiago de Compostela
Spain
;
_audit_update_record             
;
2018-07-12 deposited with the CCDC.	2019-07-23 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            'DMAPbBr_B - 6_T100K'
_chemical_formula_moiety         'Br6 Pb2, 2(C2 H8 N)'
_chemical_formula_sum            'C4 H16 Br6 N2 Pb2'
_chemical_formula_iupac          ?
_chemical_formula_weight         986.03
_chemical_absolute_configuration ad

_chemical_melting_point          ?

_space_group_crystal_system      orthorhombic
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x+1/2, -y, z+1/2'

_cell_length_a                   8.7631(4)
_cell_length_b                   13.9568(6)
_cell_length_c                   14.7110(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1799.23(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5426
_cell_measurement_theta_min      2.7052
_cell_measurement_theta_max      26.2068
_cell_measurement_temperature    100.(2)

_exptl_crystal_description       prism
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.120
_exptl_crystal_density_diffrn    3.640
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1712

_exptl_absorpt_coefficient_mu    31.990
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
'TWINABS - Bruker AXS scaling for twinned crystals - Version 2012/1'
_exptl_absorpt_correction_T_min  0.0233
_exptl_absorpt_correction_T_max  0.0613

_exptl_special_details           
;
;

_diffrn_ambient_temperature      100.(2)

_diffrn_source                   'sealed x-ray tube'
_diffrn_source_type              'SIEMENS KFN MO 2K-90'

_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device       'κ--geometry diffractometer'
_diffrn_measurement_device_type  'Bruker AXS X8 APEX-II'
_diffrn_measurement_method       'φ or ω oscillation scans'

_diffrn_detector_area_resol_mean 16.6666

_diffrn_reflns_number            23098
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.2072
_diffrn_reflns_theta_min         2.01
_diffrn_reflns_theta_max         25.41
_diffrn_reflns_theta_full        25.41
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17

_refine_special_details          'Refined as a 12-component twin.,Twin'

_reflns_number_total             23098
_reflns_number_gt                16852
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.1360
_refine_ls_R_factor_gt           0.0979
_refine_ls_wR_factor_gt          0.2229
_refine_ls_wR_factor_ref         0.2577
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.027
_refine_ls_number_reflns         23098
_refine_ls_number_parameters     142
_refine_ls_number_restraints     18
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1440P)²] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap

_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         4.214
_refine_diff_density_min         -2.844
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
;

Flack x determined using 1132 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.01(2)

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'

_computing_data_collection       'Bruker APEX3 software'
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 883)'
_computing_publication_material  ?

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb Pb1 0.2856(3) 0.31814(15) 0.37896(15) 0.0158(6) Uani d . . . 1 . .
Pb Pb2 0.3042(3) 0.33463(15) 0.11133(15) 0.0158(6) Uani d . . . 1 . .
Br Br1 0.0269(8) 0.2217(5) 0.4773(5) 0.0232(16) Uani d . . . 1 . .
Br Br2 0.2689(8) 0.4991(4) 0.4668(4) 0.0217(15) Uani d . . . 1 . .
Br Br3 0.0863(7) 0.4146(5) 0.2448(5) 0.0197(14) Uani d . . . 1 . .
Br Br4 0.5312(7) 0.3965(5) 0.2580(5) 0.0215(15) Uani d . . . 1 . .
Br Br5 0.2975(8) 0.1620(4) 0.2148(4) 0.0203(14) Uani d . . . 1 . .
Br Br6 0.0722(8) 0.2488(6) -0.0117(5) 0.0293(17) Uani d . . . 1 . .
N N11 0.297(6) 0.642(4) 0.275(3) 0.024(11) Uani d . . . 1 . .
H H11A 0.376275 0.671304 0.303479 0.029 Uiso calc U . R 1 . .
H H11B 0.286387 0.582398 0.300404 0.029 Uiso calc U . R 1 . .
C C12 0.155(7) 0.697(5) 0.293(4) 0.027(16) Uani d . . . 1 . .
H H12A 0.135488 0.699567 0.358176 0.04 Uiso calc U . R 1 . .
H H12B 0.06936 0.666519 0.261743 0.04 Uiso calc U . R 1 . .
H H12C 0.168055 0.762654 0.269432 0.04 Uiso calc U . R 1 . .
C C13 0.331(7) 0.632(4) 0.179(4) 0.022(14) Uani d . . . 1 . .
H H13A 0.242358 0.604662 0.147515 0.033 Uiso calc U . R 1 . .
H H13B 0.418803 0.589005 0.171311 0.033 Uiso calc U . R 1 . .
H H13C 0.354924 0.694743 0.153351 0.033 Uiso calc U . R 1 . .
N N21 0.683(6) 0.501(4) 0.470(4) 0.027(13) Uani d . . . 1 . .
H H21A 0.612178 0.454568 0.462442 0.033 Uiso calc U . R 1 . .
H H21B 0.651642 0.553567 0.437863 0.033 Uiso calc U . R 1 . .
C C22 0.691(9) 0.528(5) 0.569(4) 0.034(17) Uani d . . . 1 . .
H H22A 0.77749 0.570502 0.579228 0.051 Uiso calc U . R 1 . .
H H22B 0.703545 0.469314 0.605261 0.051 Uiso calc U . R 1 . .
H H22C 0.596075 0.559922 0.586654 0.051 Uiso calc U . R 1 . .
C C23 0.831(7) 0.468(5) 0.432(5) 0.030(16) Uani d . . . 1 . .
H H23A 0.912056 0.513319 0.448019 0.045 Uiso calc U . R 1 . .
H H23B 0.823547 0.462994 0.365709 0.045 Uiso calc U . R 1 . .
H H23C 0.855979 0.404638 0.457337 0.045 Uiso calc U . R 1 . .


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pb1 Br2 . 2.841(6) ?
Pb1 Br3 . 2.959(7) ?
Pb1 Br4 . 2.998(7) ?
Pb1 Br1 . 3.007(7) ?
Pb1 Br1 2_556 3.042(7) ?
Pb2 Br5 . 2.851(6) ?
Pb2 Br3 . 2.958(7) ?
Pb2 Br6 . 2.974(7) ?
Pb2 Br6 2 3.003(7) ?
Pb2 Br4 . 3.059(7) ?
Pb2 Br2 4_564 3.212(6) ?
N11 C13 . 1.46(8) ?
N11 C12 . 1.48(7) ?
N11 H11A . 0.91 ?
N11 H11B . 0.91 ?
C12 H12A . 0.98 ?
C12 H12B . 0.98 ?
C12 H12C . 0.98 ?
C13 H13A . 0.98 ?
C13 H13B . 0.98 ?
C13 H13C . 0.98 ?
N21 C23 . 1.49(8) ?
N21 C22 . 1.50(8) ?
N21 H21A . 0.91 ?
N21 H21B . 0.91 ?
C22 H22A . 0.98 ?
C22 H22B . 0.98 ?
C22 H22C . 0.98 ?
C23 H23A . 0.98 ?
C23 H23B . 0.98 ?
C23 H23C . 0.98 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Br2 Pb1 Br3 . . 82.44(19) ?
Br2 Pb1 Br4 . . 89.02(19) ?
Br3 Pb1 Br4 . . 82.08(19) ?
Br2 Pb1 Br1 . . 98.05(19) ?
Br3 Pb1 Br1 . . 94.55(19) ?
Br4 Pb1 Br1 . . 171.7(2) ?
Br2 Pb1 Br1 . 2_556 83.22(19) ?
Br3 Pb1 Br1 . 2_556 163.15(19) ?
Br4 Pb1 Br1 . 2_556 88.9(2) ?
Br1 Pb1 Br1 . 2_556 96.19(7) ?
Br5 Pb2 Br3 . . 87.19(19) ?
Br5 Pb2 Br6 . . 88.3(2) ?
Br3 Pb2 Br6 . . 96.6(2) ?
Br5 Pb2 Br6 . 2 87.1(2) ?
Br3 Pb2 Br6 . 2 167.2(2) ?
Br6 Pb2 Br6 . 2 94.67(6) ?
Br5 Pb2 Br4 . . 82.84(18) ?
Br3 Pb2 Br4 . . 81.08(18) ?
Br6 Pb2 Br4 . . 170.9(2) ?
Br6 Pb2 Br4 2 . 86.86(19) ?
Br5 Pb2 Br2 . 4_564 163.7(2) ?
Br3 Pb2 Br2 . 4_564 92.18(18) ?
Br6 Pb2 Br2 . 4_564 75.6(2) ?
Br6 Pb2 Br2 2 4_564 96.50(19) ?
Br4 Pb2 Br2 . 4_564 113.13(18) ?
Pb1 Br1 Pb1 . 2_456 160.1(2) ?
Pb1 Br2 Pb2 . 4_565 162.5(2) ?
Pb2 Br3 Pb1 . . 83.68(16) ?
Pb1 Br4 Pb2 . . 81.33(16) ?
Pb2 Br6 Pb2 . 2_455 171.0(3) ?
C13 N11 C12 . . 113.(5) ?
C13 N11 H11A . . 109.0 ?
C12 N11 H11A . . 109.0 ?
C13 N11 H11B . . 109.0 ?
C12 N11 H11B . . 109.0 ?
H11A N11 H11B . . 107.8 ?
N11 C12 H12A . . 109.5 ?
N11 C12 H12B . . 109.5 ?
H12A C12 H12B . . 109.5 ?
N11 C12 H12C . . 109.5 ?
H12A C12 H12C . . 109.5 ?
H12B C12 H12C . . 109.5 ?
N11 C13 H13A . . 109.5 ?
N11 C13 H13B . . 109.5 ?
H13A C13 H13B . . 109.5 ?
N11 C13 H13C . . 109.5 ?
H13A C13 H13C . . 109.5 ?
H13B C13 H13C . . 109.5 ?
C23 N21 C22 . . 114.(6) ?
C23 N21 H21A . . 108.8 ?
C22 N21 H21A . . 108.8 ?
C23 N21 H21B . . 108.8 ?
C22 N21 H21B . . 108.8 ?
H21A N21 H21B . . 107.7 ?
N21 C22 H22A . . 109.5 ?
N21 C22 H22B . . 109.5 ?
H22A C22 H22B . . 109.5 ?
N21 C22 H22C . . 109.5 ?
H22A C22 H22C . . 109.5 ?
H22B C22 H22C . . 109.5 ?
N21 C23 H23A . . 109.5 ?
N21 C23 H23B . . 109.5 ?
H23A C23 H23B . . 109.5 ?
N21 C23 H23C . . 109.5 ?
H23A C23 H23C . . 109.5 ?
H23B C23 H23C . . 109.5 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Br2 Pb1 Br1 Pb1 . . . 2_456 -17.5(8) ?
Br3 Pb1 Br1 Pb1 . . . 2_456 -100.5(8) ?
Br4 Pb1 Br1 Pb1 . . . 2_456 -166.1(11) ?
Br1 Pb1 Br1 Pb1 2_556 . . 2_456 66.5(8) ?
Br3 Pb1 Br2 Pb2 . . . 4_565 113.8(8) ?
Br4 Pb1 Br2 Pb2 . . . 4_565 -164.0(8) ?
Br1 Pb1 Br2 Pb2 . . . 4_565 20.3(9) ?
Br1 Pb1 Br2 Pb2 2_556 . . 4_565 -75.1(8) ?
Br5 Pb2 Br3 Pb1 . . . . 42.35(18) ?
Br6 Pb2 Br3 Pb1 . . . . 130.31(19) ?
Br6 Pb2 Br3 Pb1 2 . . . -21.1(10) ?
Br4 Pb2 Br3 Pb1 . . . . -40.83(16) ?
Br2 Pb2 Br3 Pb1 4_564 . . . -153.91(17) ?
Br2 Pb1 Br3 Pb2 . . . . 131.77(19) ?
Br4 Pb1 Br3 Pb2 . . . . 41.71(16) ?
Br1 Pb1 Br3 Pb2 . . . . -130.69(17) ?
Br1 Pb1 Br3 Pb2 2_556 . . . 99.8(7) ?
Br2 Pb1 Br4 Pb2 . . . . -122.82(18) ?
Br3 Pb1 Br4 Pb2 . . . . -40.31(16) ?
Br1 Pb1 Br4 Pb2 . . . . 26.1(15) ?
Br1 Pb1 Br4 Pb2 2_556 . . . 153.94(18) ?
Br5 Pb2 Br4 Pb1 . . . . -47.81(17) ?
Br3 Pb2 Br4 Pb1 . . . . 40.45(17) ?
Br6 Pb2 Br4 Pb1 . . . . -35.3(13) ?
Br6 Pb2 Br4 Pb1 2 . . . -135.3(2) ?
Br2 Pb2 Br4 Pb1 4_564 . . . 129.01(17) ?
Br5 Pb2 Br6 Pb2 . . . 2_455 70.(2) ?
Br3 Pb2 Br6 Pb2 . . . 2_455 -17.(2) ?
Br6 Pb2 Br6 Pb2 2 . . 2_455 157.(2) ?
Br4 Pb2 Br6 Pb2 . . . 2_455 57.(3) ?
Br2 Pb2 Br6 Pb2 4_564 . . 2_455 -108.(2) ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N11 H11B Br2 . 0.91 2.71 3.46(5) 139.4 ?
N11 H11B Br3 . 0.91 3.04 3.69(5) 130.5 ?
N11 H11B Br4 . 0.91 3.42 4.00(5) 123.7 ?
N11 H11A Br4 3_655 0.91 3.37 3.89(5) 119.1 ?
N11 H11A Br5 3_655 0.91 2.87 3.57(5) 134.5 ?
N11 H11A Br6 4_565 0.91 2.97 3.67(5) 134.5 ?
N21 H21A Br1 2_556 0.91 2.72 3.49(5) 143.0 ?
N21 H21A Br2 . 0.91 3.07 3.63(6) 121.4 ?
N21 H21A Br4 . 0.91 3.19 3.69(6) 116.7 ?
N21 H21B Br5 3_655 0.91 2.74 3.53(5) 144.7 ?
N21 H21B Br6 4_565 0.91 3.47 4.15(5) 134.2 ?


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: DMF'
