# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1886424'
loop_
_audit_author_name
_audit_author_address
'Maroua Ben Haj Salah'
;University of Angers
France
;
_audit_update_record             
;
2018-12-20 deposited with the CCDC.	2019-03-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Br10 Pb2, 3(C6 H16 N2 O2), 3(O)'
_chemical_formula_sum            'C18 H48 Br10 N6 O9 Pb2'
_chemical_formula_weight         1706.02
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -4.0753 8.5060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_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'

_cell_length_a                   8.1393(3)
_cell_length_b                   25.2015(9)
_cell_length_c                   10.9881(5)
_cell_angle_alpha                90
_cell_angle_beta                 91.088(3)
_cell_angle_gamma                90
_cell_volume                     2253.50(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    150.00(10)
_cell_measurement_reflns_used    3127
_cell_measurement_theta_min      3.4460
_cell_measurement_theta_max      72.0410

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.514
_exptl_crystal_F_000             1568
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    25.119
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.81661
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41r (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      149.9(3)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova(Cu) micro-focus sealed X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Single source at offset, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.1990
_diffrn_reflns_number            9248
_diffrn_reflns_av_unetI/netI     0.1128
_diffrn_reflns_av_R_equivalents  0.0636
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.508
_diffrn_reflns_theta_max         72.633
_diffrn_reflns_theta_full        69.000
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.749
_diffrn_reflns_point_group_measured_fraction_full 0.776
_reflns_number_total             6698
_reflns_number_gt                5742
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.505
_reflns_Friedel_fraction_max     0.515
_reflns_Friedel_fraction_full    0.546

_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       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    'DIAMOND 3.2k (Crystal Impact GbR, 2014)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_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)+(0.0777P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2016/4 (Sheldrick 2016)'
_refine_ls_extinction_coef       0.00007(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.023(15)
_chemical_absolute_configuration syn
_refine_ls_number_reflns         6698
_refine_ls_number_parameters     404
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0576
_refine_ls_wR_factor_ref         0.1516
_refine_ls_wR_factor_gt          0.1458
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_restrained_S_all      1.013
_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
C1 C 1.233(4) -0.3206(13) 0.749(3) 0.047(7) Uani 1 1 d . . . . .
H1A H 1.275313 -0.285180 0.734945 0.057 Uiso 1 1 calc R U . . .
H1B H 1.325848 -0.344473 0.759407 0.057 Uiso 1 1 calc R U . . .
C2 C 1.130(4) -0.3209(11) 0.865(3) 0.042(6) Uani 1 1 d . . . . .
H2A H 1.100655 -0.356965 0.886652 0.051 Uiso 1 1 calc R U . . .
H2B H 1.028929 -0.300901 0.851601 0.051 Uiso 1 1 calc R U . . .
C3 C 1.233(4) -0.2952(11) 0.969(3) 0.043(6) Uani 1 1 d . . . . .
H3A H 1.284338 -0.262784 0.940752 0.052 Uiso 1 1 calc R U . . .
H3B H 1.319159 -0.319337 0.996445 0.052 Uiso 1 1 calc R U . . .
C4 C 1.114(3) -0.2828(10) 1.076(2) 0.037(5) Uani 1 1 d . . . . .
H4A H 1.028700 -0.259070 1.045766 0.045 Uiso 1 1 calc R U . . .
H4B H 1.062209 -0.315493 1.100569 0.045 Uiso 1 1 calc R U . . .
C5 C 1.198(4) -0.2577(12) 1.185(2) 0.040(6) Uani 1 1 d . . . . .
H5 H 1.115150 -0.245279 1.242357 0.049 Uiso 1 1 calc R U . . .
C6 C 1.305(3) -0.2106(11) 1.144(2) 0.035(5) Uani 1 1 d . . . . .
C7 C 0.093(3) 0.4032(15) 0.980(3) 0.052(8) Uani 1 1 d . . . . .
H7A H 0.063130 0.366581 0.995815 0.062 Uiso 1 1 calc R U . . .
H7B H -0.006002 0.422655 0.958276 0.062 Uiso 1 1 calc R U . . .
C8 C 0.212(4) 0.4056(16) 0.879(3) 0.053(8) Uani 1 1 d . . . . .
H8A H 0.317349 0.392339 0.907107 0.064 Uiso 1 1 calc R U . . .
H8B H 0.226002 0.442333 0.854480 0.064 Uiso 1 1 calc R U . . .
C9 C 0.155(3) 0.3732(14) 0.767(3) 0.046(6) Uani 1 1 d . . . . .
H9A H 0.123997 0.337757 0.792929 0.056 Uiso 1 1 calc R U . . .
H9B H 0.058538 0.389810 0.730143 0.056 Uiso 1 1 calc R U . . .
C10 C 0.286(3) 0.3699(13) 0.678(3) 0.045(6) Uani 1 1 d . . . . .
H10A H 0.380214 0.353064 0.717095 0.054 Uiso 1 1 calc R U . . .
H10B H 0.317569 0.405632 0.656477 0.054 Uiso 1 1 calc R U . . .
C11 C 0.243(4) 0.3393(11) 0.561(3) 0.042(6) Uani 1 1 d . . . . .
H11 H 0.342494 0.335370 0.513251 0.051 Uiso 1 1 calc R U . . .
C12 C 0.169(4) 0.2835(15) 0.583(3) 0.052(7) Uani 1 1 d . . . . .
C13 C 0.691(3) 0.6417(10) 0.078(2) 0.035(5) Uani 1 1 d . . . . .
C14 C 0.737(4) 0.5828(12) 0.087(2) 0.041(6) Uani 1 1 d . . . . .
H14 H 0.848399 0.581340 0.122150 0.049 Uiso 1 1 calc R U . . .
C15 C 0.744(3) 0.5564(11) -0.035(2) 0.040(6) Uani 1 1 d . . . . .
H15A H 0.769329 0.519133 -0.022637 0.048 Uiso 1 1 calc R U . . .
H15B H 0.832976 0.571999 -0.079951 0.048 Uiso 1 1 calc R U . . .
C16 C 0.584(3) 0.5610(17) -0.111(2) 0.055(9) Uani 1 1 d . . . . .
H16A H 0.509345 0.533467 -0.084705 0.066 Uiso 1 1 calc R U . . .
H16B H 0.533619 0.594903 -0.093127 0.066 Uiso 1 1 calc R U . . .
C17 C 0.602(6) 0.557(2) -0.244(4) 0.081(12) Uani 1 1 d . . . . .
H17A H 0.689893 0.580028 -0.268837 0.097 Uiso 1 1 calc R U . . .
H17B H 0.501390 0.568350 -0.283541 0.097 Uiso 1 1 calc R U . . .
C18 C 0.640(5) 0.5008(15) -0.284(3) 0.062(9) Uani 1 1 d . . . . .
H18A H 0.544512 0.478408 -0.274144 0.075 Uiso 1 1 calc R U . . .
H18B H 0.729563 0.486370 -0.234689 0.075 Uiso 1 1 calc R U . . .
N1 N 1.130(4) -0.3377(13) 0.643(2) 0.059(7) Uani 1 1 d . . . . .
H1C H 1.190038 -0.337521 0.576617 0.089 Uiso 1 1 calc R U . . .
H1D H 1.092442 -0.370332 0.656527 0.089 Uiso 1 1 calc R U . . .
H1E H 1.045710 -0.315502 0.633906 0.089 Uiso 1 1 calc R U . . .
N2 N 1.308(3) -0.2964(10) 1.246(2) 0.048(6) Uani 1 1 d . . . . .
H2C H 1.356839 -0.281242 1.310402 0.071 Uiso 1 1 calc R U . . .
H2D H 1.250440 -0.324329 1.269925 0.071 Uiso 1 1 calc R U . . .
H2E H 1.384553 -0.306909 1.194139 0.071 Uiso 1 1 calc R U . . .
N3 N 0.175(3) 0.4278(12) 1.094(2) 0.050(6) Uani 1 1 d . . . . .
H3C H 0.105663 0.426565 1.155878 0.075 Uiso 1 1 calc R U . . .
H3D H 0.265547 0.409544 1.113974 0.075 Uiso 1 1 calc R U . . .
H3E H 0.201681 0.461347 1.079294 0.075 Uiso 1 1 calc R U . . .
N4 N 0.121(3) 0.3692(11) 0.489(2) 0.049(5) Uani 1 1 d . . . . .
H4C H 0.096662 0.351488 0.420886 0.073 Uiso 1 1 calc R U . . .
H4D H 0.030888 0.373679 0.531905 0.073 Uiso 1 1 calc R U . . .
H4E H 0.162785 0.400796 0.469850 0.073 Uiso 1 1 calc R U . . .
N5 N 0.631(3) 0.5574(8) 0.1743(16) 0.034(4) Uani 1 1 d . . . . .
H5A H 0.633505 0.575484 0.243787 0.051 Uiso 1 1 calc R U . . .
H5B H 0.528135 0.556656 0.144632 0.051 Uiso 1 1 calc R U . . .
H5C H 0.665146 0.524333 0.187820 0.051 Uiso 1 1 calc R U . . .
N6 N 0.688(3) 0.5017(9) -0.4173(18) 0.041(5) Uani 1 1 d . . . . .
H6A H 0.710969 0.468852 -0.441614 0.062 Uiso 1 1 calc R U . . .
H6B H 0.605781 0.514701 -0.462271 0.062 Uiso 1 1 calc R U . . .
H6C H 0.776838 0.522061 -0.425800 0.062 Uiso 1 1 calc R U . . .
O1 O 1.457(3) -0.2115(9) 1.149(2) 0.048(5) Uani 1 1 d . . . . .
O2 O 1.219(2) -0.1719(7) 1.1026(18) 0.043(4) Uani 1 1 d . . . . .
H2 H 1.121429 -0.179473 1.105870 0.064 Uiso 1 1 calc R U . . .
O3 O 0.277(3) 0.2506(11) 0.628(3) 0.068(7) Uani 1 1 d . . . . .
H3 H 0.365637 0.265789 0.636094 0.102 Uiso 1 1 calc R U . . .
O4 O 0.028(3) 0.2742(10) 0.557(3) 0.065(6) Uani 1 1 d . . . . .
O5 O 0.591(3) 0.6599(9) 0.146(2) 0.053(5) Uani 1 1 d . . . . .
O6 O 0.771(3) 0.6659(10) -0.0006(19) 0.052(5) Uani 1 1 d . . . . .
H6 H 0.742890 0.697121 -0.002315 0.078 Uiso 1 1 calc R U . . .
O7 O 0.714(2) 0.7682(8) 0.9946(12) 0.052(5) Uani 1 1 d G . . . .
O8 O 0.302(2) 0.7393(9) 0.4891(16) 0.051(5) Uani 1 1 d G . . . .
O9 O 0.786(2) 0.6776(10) 0.6451(17) 0.067(6) Uani 1 1 d G . . . .
BR1 Br 0.6061(3) -0.04654(10) 0.6323(3) 0.0381(6) Uani 1 1 d . . . . .
BR2 Br 0.5638(4) -0.21319(13) 0.7123(3) 0.0479(7) Uani 1 1 d . . . . .
BR3 Br 0.5274(3) 0.10948(10) 0.5548(2) 0.0346(5) Uani 1 1 d . . . . .
BR4 Br 1.1038(3) -0.02728(10) 0.6869(2) 0.0348(5) Uani 1 1 d . . . . .
BR5 Br 1.0535(3) 0.13982(11) 0.6434(3) 0.0398(6) Uani 1 1 d . . . . .
BR6 Br 0.7788(3) 0.06199(11) 0.8907(2) 0.0404(6) Uani 1 1 d . . . . .
BR7 Br 0.2761(3) -0.12951(12) 0.4294(2) 0.0420(6) Uani 1 1 d . . . . .
BR8 Br 0.8995(5) 0.02622(16) 0.3577(3) 0.0594(9) Uani 1 1 d . . . . .
BR9 Br 0.0374(3) -0.18200(12) 0.7687(3) 0.0473(7) Uani 1 1 d . . . . .
BR11 Br 0.4001(4) -0.08143(12) 0.9534(3) 0.0446(6) Uani 1 1 d . . . . .
PB1 Pb 0.82525(10) 0.04808(3) 0.61880(8) 0.0293(2) Uani 1 1 d . . . . .
PB2 Pb 0.32676(11) -0.12346(3) 0.70490(8) 0.0326(2) 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 N1 1.48(4) . ?
C1 C2 1.54(4) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 C3 1.55(4) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.56(4) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.51(4) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 N2 1.48(3) . ?
C5 C6 1.55(4) . ?
C5 H5 0.9800 . ?
C6 O1 1.23(3) . ?
C6 O2 1.28(3) . ?
C7 C8 1.49(4) . ?
C7 N3 1.54(4) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C9 1.53(4) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.46(4) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.54(4) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 N4 1.46(4) . ?
C11 C12 1.55(5) . ?
C11 H11 0.9800 . ?
C12 O4 1.20(4) . ?
C12 O3 1.30(4) . ?
C13 O5 1.21(3) . ?
C13 O6 1.25(3) . ?
C13 C14 1.53(4) . ?
C14 N5 1.45(3) . ?
C14 C15 1.50(4) . ?
C14 H14 0.9800 . ?
C15 C16 1.54(4) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.47(5) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.51(6) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 N6 1.52(4) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
N1 H1C 0.8900 . ?
N1 H1D 0.8900 . ?
N1 H1E 0.8900 . ?
N2 H2C 0.8900 . ?
N2 H2D 0.8900 . ?
N2 H2E 0.8900 . ?
N3 H3C 0.8900 . ?
N3 H3D 0.8900 . ?
N3 H3E 0.8900 . ?
N4 H4C 0.8900 . ?
N4 H4D 0.8900 . ?
N4 H4E 0.8900 . ?
N5 H5A 0.8900 . ?
N5 H5B 0.8900 . ?
N5 H5C 0.8900 . ?
N6 H6A 0.8900 . ?
N6 H6B 0.8900 . ?
N6 H6C 0.8900 . ?
O2 H2 0.8200 . ?
O3 H3 0.8200 . ?
O6 H6 0.8200 . ?
BR1 PB1 2.983(3) . ?
BR1 PB2 3.104(3) . ?
BR2 PB2 2.973(3) . ?
BR3 PB1 2.950(3) . ?
BR4 PB2 3.032(3) 1_655 ?
BR4 PB1 3.040(3) . ?
BR5 PB1 2.975(3) . ?
BR6 PB1 3.039(3) . ?
BR7 PB2 3.051(3) . ?
BR8 PB1 2.994(3) . ?
BR9 PB2 2.877(3) . ?
BR11 PB2 2.978(3) . ?
PB2 BR4 3.032(3) 1_455 ?

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
N1 C1 C2 110(2) . . ?
N1 C1 H1A 109.7 . . ?
C2 C1 H1A 109.7 . . ?
N1 C1 H1B 109.7 . . ?
C2 C1 H1B 109.7 . . ?
H1A C1 H1B 108.2 . . ?
C1 C2 C3 108(2) . . ?
C1 C2 H2A 110.1 . . ?
C3 C2 H2A 110.1 . . ?
C1 C2 H2B 110.1 . . ?
C3 C2 H2B 110.1 . . ?
H2A C2 H2B 108.4 . . ?
C2 C3 C4 107(2) . . ?
C2 C3 H3A 110.2 . . ?
C4 C3 H3A 110.2 . . ?
C2 C3 H3B 110.2 . . ?
C4 C3 H3B 110.2 . . ?
H3A C3 H3B 108.5 . . ?
C5 C4 C3 114(2) . . ?
C5 C4 H4A 108.8 . . ?
C3 C4 H4A 108.8 . . ?
C5 C4 H4B 108.8 . . ?
C3 C4 H4B 108.8 . . ?
H4A C4 H4B 107.7 . . ?
N2 C5 C4 110(2) . . ?
N2 C5 C6 107(2) . . ?
C4 C5 C6 109(2) . . ?
N2 C5 H5 110.0 . . ?
C4 C5 H5 110.0 . . ?
C6 C5 H5 110.0 . . ?
O1 C6 O2 125(3) . . ?
O1 C6 C5 123(2) . . ?
O2 C6 C5 112(2) . . ?
C8 C7 N3 108(2) . . ?
C8 C7 H7A 110.0 . . ?
N3 C7 H7A 110.0 . . ?
C8 C7 H7B 110.0 . . ?
N3 C7 H7B 110.0 . . ?
H7A C7 H7B 108.4 . . ?
C7 C8 C9 113(3) . . ?
C7 C8 H8A 109.1 . . ?
C9 C8 H8A 109.1 . . ?
C7 C8 H8B 109.1 . . ?
C9 C8 H8B 109.1 . . ?
H8A C8 H8B 107.8 . . ?
C10 C9 C8 110(2) . . ?
C10 C9 H9A 109.6 . . ?
C8 C9 H9A 109.6 . . ?
C10 C9 H9B 109.6 . . ?
C8 C9 H9B 109.6 . . ?
H9A C9 H9B 108.1 . . ?
C9 C10 C11 116(2) . . ?
C9 C10 H10A 108.4 . . ?
C11 C10 H10A 108.4 . . ?
C9 C10 H10B 108.4 . . ?
C11 C10 H10B 108.4 . . ?
H10A C10 H10B 107.4 . . ?
N4 C11 C10 110(2) . . ?
N4 C11 C12 107(2) . . ?
C10 C11 C12 114(2) . . ?
N4 C11 H11 108.7 . . ?
C10 C11 H11 108.7 . . ?
C12 C11 H11 108.7 . . ?
O4 C12 O3 127(3) . . ?
O4 C12 C11 121(3) . . ?
O3 C12 C11 112(3) . . ?
O5 C13 O6 128(3) . . ?
O5 C13 C14 119(3) . . ?
O6 C13 C14 113(2) . . ?
N5 C14 C15 115(2) . . ?
N5 C14 C13 109(2) . . ?
C15 C14 C13 113(2) . . ?
N5 C14 H14 106.4 . . ?
C15 C14 H14 106.4 . . ?
C13 C14 H14 106.4 . . ?
C14 C15 C16 114(2) . . ?
C14 C15 H15A 108.8 . . ?
C16 C15 H15A 108.8 . . ?
C14 C15 H15B 108.8 . . ?
C16 C15 H15B 108.8 . . ?
H15A C15 H15B 107.6 . . ?
C17 C16 C15 116(3) . . ?
C17 C16 H16A 108.3 . . ?
C15 C16 H16A 108.3 . . ?
C17 C16 H16B 108.3 . . ?
C15 C16 H16B 108.3 . . ?
H16A C16 H16B 107.4 . . ?
C16 C17 C18 113(4) . . ?
C16 C17 H17A 109.0 . . ?
C18 C17 H17A 109.0 . . ?
C16 C17 H17B 109.0 . . ?
C18 C17 H17B 109.0 . . ?
H17A C17 H17B 107.8 . . ?
C17 C18 N6 109(3) . . ?
C17 C18 H18A 109.9 . . ?
N6 C18 H18A 109.9 . . ?
C17 C18 H18B 109.9 . . ?
N6 C18 H18B 109.9 . . ?
H18A C18 H18B 108.3 . . ?
C1 N1 H1C 109.5 . . ?
C1 N1 H1D 109.5 . . ?
H1C N1 H1D 109.5 . . ?
C1 N1 H1E 109.5 . . ?
H1C N1 H1E 109.5 . . ?
H1D N1 H1E 109.5 . . ?
C5 N2 H2C 109.5 . . ?
C5 N2 H2D 109.5 . . ?
H2C N2 H2D 109.5 . . ?
C5 N2 H2E 109.5 . . ?
H2C N2 H2E 109.5 . . ?
H2D N2 H2E 109.5 . . ?
C7 N3 H3C 109.5 . . ?
C7 N3 H3D 109.5 . . ?
H3C N3 H3D 109.5 . . ?
C7 N3 H3E 109.5 . . ?
H3C N3 H3E 109.5 . . ?
H3D N3 H3E 109.5 . . ?
C11 N4 H4C 109.5 . . ?
C11 N4 H4D 109.5 . . ?
H4C N4 H4D 109.5 . . ?
C11 N4 H4E 109.5 . . ?
H4C N4 H4E 109.5 . . ?
H4D N4 H4E 109.5 . . ?
C14 N5 H5A 109.5 . . ?
C14 N5 H5B 109.5 . . ?
H5A N5 H5B 109.5 . . ?
C14 N5 H5C 109.5 . . ?
H5A N5 H5C 109.5 . . ?
H5B N5 H5C 109.5 . . ?
C18 N6 H6A 109.5 . . ?
C18 N6 H6B 109.5 . . ?
H6A N6 H6B 109.5 . . ?
C18 N6 H6C 109.5 . . ?
H6A N6 H6C 109.5 . . ?
H6B N6 H6C 109.5 . . ?
C6 O2 H2 109.5 . . ?
C12 O3 H3 109.5 . . ?
C13 O6 H6 109.5 . . ?
PB1 BR1 PB2 162.48(11) . . ?
PB2 BR4 PB1 163.34(10) 1_655 . ?
BR3 PB1 BR5 97.06(8) . . ?
BR3 PB1 BR1 86.65(8) . . ?
BR5 PB1 BR1 171.74(8) . . ?
BR3 PB1 BR8 92.75(8) . . ?
BR5 PB1 BR8 95.33(10) . . ?
BR1 PB1 BR8 91.84(10) . . ?
BR3 PB1 BR6 93.26(8) . . ?
BR5 PB1 BR6 84.86(8) . . ?
BR1 PB1 BR6 87.58(8) . . ?
BR8 PB1 BR6 173.92(9) . . ?
BR3 PB1 BR4 172.77(8) . . ?
BR5 PB1 BR4 90.09(8) . . ?
BR1 PB1 BR4 86.12(8) . . ?
BR8 PB1 BR4 87.58(9) . . ?
BR6 PB1 BR4 86.34(8) . . ?
BR9 PB2 BR2 97.88(9) . . ?
BR9 PB2 BR11 96.30(9) . . ?
BR2 PB2 BR11 97.28(10) . . ?
BR9 PB2 BR4 86.23(8) . 1_455 ?
BR2 PB2 BR4 175.73(9) . 1_455 ?
BR11 PB2 BR4 83.38(8) . 1_455 ?
BR9 PB2 BR7 96.91(9) . . ?
BR2 PB2 BR7 93.71(9) . . ?
BR11 PB2 BR7 161.48(9) . . ?
BR4 PB2 BR7 84.59(8) 1_455 . ?
BR9 PB2 BR1 171.88(9) . . ?
BR2 PB2 BR1 90.23(8) . . ?
BR11 PB2 BR1 83.03(8) . . ?
BR4 PB2 BR1 85.66(8) 1_455 . ?
BR7 PB2 BR1 82.06(8) . . ?

_refine_diff_density_max         2.190
_refine_diff_density_min         -2.268
_refine_diff_density_rms         0.287

####################################################################### 
# 
# 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_shelx_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1886427'
loop_
_audit_author_name
_audit_author_address
'Maroua Ben Haj Salah'
;University of Angers
France
;
_audit_update_record             
;
2018-12-20 deposited with the CCDC.	2019-03-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Br14 Pb3, 4(C5 H15 N2 O2), 2(H2 O)'
_chemical_formula_sum            'C20 H64 Br14 N8 O10 Pb3 '
_chemical_formula_weight         2316.99

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -4.0753 8.5060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_H-M_alt        'P 1'
_space_group_name_Hall           'P 1'

_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'

_cell_length_a                   8.274(5)
_cell_length_b                   11.580(5)
_cell_length_c                   15.717(5)
_cell_angle_alpha                71.769(5)
_cell_angle_beta                 77.947(5)
_cell_angle_gamma                72.105(5)
_cell_volume                     1350.5(11)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(10)
_cell_measurement_reflns_used    15738
_cell_measurement_theta_min      2.9310
_cell_measurement_theta_max      72.3910

_exptl_crystal_description       plate
_exptl_crystal_colour            transparent
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.849
_exptl_crystal_F_000             1056
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    30.423
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.61273
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41r (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      149.9(3)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova(Cu) micro-focus sealed X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Single source at offset, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.1990

_diffrn_reflns_number            22457
_diffrn_reflns_av_unetI/netI     0.0554
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.983
_diffrn_reflns_theta_max         72.610
_diffrn_reflns_theta_full        70.000
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.908
_diffrn_reflns_point_group_measured_fraction_full 0.930
_reflns_number_total             9754
_reflns_number_gt                9289
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.849
_reflns_Friedel_fraction_max     0.834
_reflns_Friedel_fraction_full    0.865

_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      'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    'DIAMOND 3.2k (Crystal Impact GbR, 2014)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'


_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)+(0.0330P)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     'SHELXL-2016/4 (Sheldrick 2016)'
_refine_ls_extinction_coef       0.00015(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 3890 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.011(7)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         9754
_refine_ls_number_parameters     494
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0306
_refine_ls_wR_factor_ref         0.0745
_refine_ls_wR_factor_gt          0.0738
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.015
_refine_ls_shift/su_max          0.001
_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 0.6398(19) 0.7683(14) 0.1533(9) 0.027(3) Uani 1 1 d . . . . .
H1A H 0.745532 0.794006 0.132425 0.032 Uiso 1 1 calc R U . . .
H1B H 0.571616 0.800592 0.103551 0.032 Uiso 1 1 calc R U . . .
C2 C 0.6797(17) 0.6263(12) 0.1825(8) 0.019(2) Uani 1 1 d . . . . .
H2A H 0.573860 0.600890 0.203989 0.022 Uiso 1 1 calc R U . . .
H2B H 0.748392 0.594268 0.232075 0.022 Uiso 1 1 calc R U . . .
C3 C 0.776(2) 0.5698(15) 0.1051(10) 0.029(3) Uani 1 1 d . . . . .
H3A H 0.882602 0.594424 0.084668 0.034 Uiso 1 1 calc R U . . .
H3B H 0.708244 0.604124 0.055178 0.034 Uiso 1 1 calc R U . . .
C4 C 0.8158(15) 0.4259(14) 0.1312(9) 0.023(3) Uani 1 1 d . . . . .
H4 H 0.874676 0.389565 0.185232 0.028 Uiso 1 1 calc R U . . .
C5 C 0.6519(17) 0.3845(13) 0.1471(11) 0.027(3) Uani 1 1 d . . . . .
H5 H 0.719057 0.297350 0.151219 0.032 Uiso 1 1 calc R U . . .
C6 C 0.0276(18) 0.4438(14) 0.6648(10) 0.031(3) Uani 1 1 d . . . . .
H6A H -0.042313 0.397899 0.653393 0.037 Uiso 1 1 calc R U . . .
H6B H 0.016494 0.430896 0.729599 0.037 Uiso 1 1 calc R U . . .
C7 C 0.2117(16) 0.3926(14) 0.6306(9) 0.026(3) Uani 1 1 d . . . . .
H7A H 0.281183 0.440062 0.640370 0.031 Uiso 1 1 calc R U . . .
H7B H 0.222254 0.402933 0.566172 0.031 Uiso 1 1 calc R U . . .
C8 C 0.2769(16) 0.2551(15) 0.6777(10) 0.025(3) Uani 1 1 d . . . . .
H8A H 0.254645 0.243862 0.742448 0.030 Uiso 1 1 calc R U . . .
H8B H 0.399809 0.229105 0.661600 0.030 Uiso 1 1 calc R U . . .
C9 C 0.1931(15) 0.1713(12) 0.6528(8) 0.020(2) Uani 1 1 d . . . . .
H9 H 0.072018 0.215903 0.649266 0.024 Uiso 1 1 calc R U . . .
C10 C 0.2703(15) 0.1458(13) 0.5603(8) 0.019(3) Uani 1 1 d . . . . .
H10 H 0.366763 0.079237 0.586404 0.023 Uiso 1 1 calc R U . . .
C11 C 0.4861(15) 0.2325(12) 0.8901(8) 0.020(2) Uani 1 1 d . . . . .
H11A H 0.507779 0.240206 0.825766 0.024 Uiso 1 1 calc R U . . .
H11B H 0.377497 0.211328 0.912742 0.024 Uiso 1 1 calc R U . . .
C12 C 0.4752(15) 0.3547(12) 0.9058(9) 0.020(2) Uani 1 1 d . . . . .
H12A H 0.576528 0.382753 0.875258 0.024 Uiso 1 1 calc R U . . .
H12B H 0.469774 0.344537 0.969935 0.024 Uiso 1 1 calc R U . . .
C13 C 0.3150(16) 0.4533(13) 0.8701(9) 0.019(3) Uani 1 1 d . . . . .
H13A H 0.329779 0.471348 0.804759 0.023 Uiso 1 1 calc R U . . .
H13B H 0.217402 0.417823 0.893074 0.023 Uiso 1 1 calc R U . . .
C14 C 0.2764(15) 0.5755(12) 0.8956(8) 0.019(2) Uani 1 1 d . . . . .
H14 H 0.163793 0.625239 0.877439 0.023 Uiso 1 1 calc R U . . .
C15 C 0.2631(15) 0.5588(13) 0.9960(9) 0.022(3) Uani 1 1 d . . . . .
H15 H 0.371711 0.493365 0.999669 0.027 Uiso 1 1 calc R U . . .
C16 C -0.0937(19) 0.9766(14) 0.4137(9) 0.026(3) Uani 1 1 d . . . . .
H16A H -0.196872 0.947279 0.432358 0.031 Uiso 1 1 calc R U . . .
H16B H -0.024660 0.940182 0.463139 0.031 Uiso 1 1 calc R U . . .
C17 C -0.1411(17) 1.1164(13) 0.3940(8) 0.022(3) Uani 1 1 d . . . . .
H17A H -0.227536 1.153028 0.353110 0.026 Uiso 1 1 calc R U . . .
H17B H -0.041382 1.147716 0.365376 0.026 Uiso 1 1 calc R U . . .
C18 C -0.2093(16) 1.1537(12) 0.4812(8) 0.018(2) Uani 1 1 d . U . . .
H18A H -0.121017 1.116374 0.521086 0.021 Uiso 1 1 calc R U . . .
H18B H -0.305602 1.118361 0.510120 0.021 Uiso 1 1 calc R U . . .
C19 C -0.2681(15) 1.2980(12) 0.4707(9) 0.019(2) Uani 1 1 d . . . . .
H19 H -0.294356 1.312783 0.530811 0.023 Uiso 1 1 calc R U . . .
C20 C -0.1260(17) 1.3571(12) 0.4179(9) 0.021(3) Uani 1 1 d . . . . .
H20 H -0.192010 1.438338 0.428933 0.025 Uiso 1 1 calc R U . . .
N1 N 0.5462(17) 0.8210(13) 0.2281(8) 0.030(3) Uani 1 1 d . . . . .
H1C H 0.523718 0.904598 0.209813 0.045 Uiso 1 1 calc R U . . .
H1D H 0.448526 0.798287 0.246720 0.045 Uiso 1 1 calc R U . . .
H1E H 0.609484 0.792191 0.273442 0.045 Uiso 1 1 calc R U . . .
N2 N 0.9228(15) 0.3784(12) 0.0551(8) 0.028(2) Uani 1 1 d . . . . .
H2C H 1.020943 0.400283 0.042939 0.042 Uiso 1 1 calc R U . . .
H2D H 0.944353 0.294818 0.069930 0.042 Uiso 1 1 calc R U . . .
H2E H 0.867490 0.411317 0.006592 0.042 Uiso 1 1 calc R U . . .
N3 N -0.0365(17) 0.5811(13) 0.6205(9) 0.029(3) Uani 1 1 d . . . . .
H3C H -0.145374 0.608315 0.642209 0.044 Uiso 1 1 calc R U . . .
H3D H 0.026189 0.623602 0.631771 0.044 Uiso 1 1 calc R U . . .
H3E H -0.028289 0.593034 0.561175 0.044 Uiso 1 1 calc R U . . .
N4 N 0.2005(15) 0.0489(12) 0.7230(8) 0.024(2) Uani 1 1 d . . . . .
H4A H 0.150657 0.002908 0.706194 0.035 Uiso 1 1 calc R U . . .
H4B H 0.309305 0.007480 0.729335 0.035 Uiso 1 1 calc R U . . .
H4C H 0.146071 0.063222 0.775353 0.035 Uiso 1 1 calc R U . . .
N5 N 0.6251(14) 0.1294(12) 0.9359(8) 0.022(2) Uani 1 1 d . . . . .
H5A H 0.628623 0.057463 0.925309 0.033 Uiso 1 1 calc R U . . .
H5B H 0.725075 0.148045 0.914495 0.033 Uiso 1 1 calc R U . . .
H5C H 0.604416 0.121300 0.995047 0.033 Uiso 1 1 calc R U . . .
N6 N 0.4008(16) 0.6516(11) 0.8442(9) 0.025(2) Uani 1 1 d G . . . .
H6C H 0.406829 0.660398 0.785431 0.037 Uiso 1 1 calc R U . . .
H6D H 0.365598 0.727216 0.854755 0.037 Uiso 1 1 calc R U . . .
H6E H 0.503718 0.612410 0.862049 0.037 Uiso 1 1 calc R U . . .
N7 N 0.0047(17) 0.9329(12) 0.3324(9) 0.029(3) Uani 1 1 d . . . . .
H7C H 0.031127 0.849185 0.346136 0.044 Uiso 1 1 calc R U . . .
H7D H -0.059129 0.965084 0.287190 0.044 Uiso 1 1 calc R U . . .
H7E H 0.100379 0.958510 0.315700 0.044 Uiso 1 1 calc R U . . .
N8 N -0.4206(13) 1.3604(11) 0.4228(8) 0.024(2) Uani 1 1 d . . . . .
H8C H -0.506423 1.326931 0.452844 0.036 Uiso 1 1 calc R U . . .
H8D H -0.450746 1.442337 0.419094 0.036 Uiso 1 1 calc R U . . .
H8E H -0.396618 1.349538 0.367453 0.036 Uiso 1 1 calc R U . . .
O1 O 0.5886(16) 0.3849(13) 0.0847(9) 0.043(3) Uani 1 1 d . . . . .
H1 H 0.501590 0.360288 0.103858 0.064 Uiso 1 1 calc R U . . .
O2 O 0.5903(13) 0.3521(11) 0.2325(8) 0.037(2) Uani 1 1 d . . . . .
O3 O 0.3659(13) 0.2035(10) 0.5071(7) 0.030(2) Uani 1 1 d . . . . .
O4 O 0.2089(12) 0.0648(10) 0.5450(7) 0.025(2) Uani 1 1 d . . . . .
H4D H 0.139837 0.042356 0.588102 0.038 Uiso 1 1 calc R U . . .
O5 O 0.1890(12) 0.4867(10) 1.0504(6) 0.026(2) Uani 1 1 d . . . . .
O6 O 0.3308(12) 0.6342(9) 1.0152(7) 0.025(2) Uani 1 1 d . . . . .
H6 H 0.369571 0.678251 0.968348 0.038 Uiso 1 1 calc R U . . .
O7 O -0.1209(12) 1.4042(9) 0.3367(6) 0.028(2) Uani 1 1 d . . . . .
H7 H -0.203098 1.397478 0.318881 0.042 Uiso 1 1 calc R U . . .
O8 O -0.0079(14) 1.3510(11) 0.4653(8) 0.032(2) Uani 1 1 d . . . . .
O9 O 0.2283(12) 1.4412(9) 0.3534(7) 0.028(2) Uiso 1 1 d G . . . .
H9A H 0.149440 1.414312 0.346058 0.10(10) Uiso 1 1 d G . . . .
H9B H 0.275491 1.389873 0.398679 0.04(5) Uiso 1 1 d G . . . .
O10 O 0.3080(15) 0.2933(9) 0.2318(8) 0.042(3) Uiso 1 1 d G . . . .
H1OA H 0.321435 0.242048 0.200825 0.2(2) Uiso 1 1 d G . . . .
H10B H 0.228989 0.358252 0.211872 0.02(4) Uiso 1 1 d G . . . .
BR1 Br 0.2711(2) 1.10375(15) 0.11489(11) 0.0307(3) Uani 1 1 d . . . . .
BR2 Br 0.45002(18) 0.91467(15) -0.10355(9) 0.0212(3) Uani 1 1 d . . . . .
BR3 Br 0.1932(2) 0.72607(15) 0.19215(10) 0.0307(3) Uani 1 1 d . . . . .
BR4 Br 0.00377(18) 1.20309(14) -0.10061(10) 0.0227(3) Uani 1 1 d . . . . .
BR5 Br -0.20711(18) 1.05520(16) 0.14590(10) 0.0283(4) Uani 1 1 d . . . . .
BR6 Br -0.04151(18) 0.85154(14) -0.06282(10) 0.0241(3) Uani 1 1 d . . . . .
BR7 Br 0.13821(18) 0.77716(15) -0.32357(9) 0.0224(3) Uani 1 1 d . . . . .
BR8 Br -0.22010(17) 1.11869(14) -0.28448(9) 0.0230(3) Uani 1 1 d . . . . .
BR9 Br -0.18520(19) 0.57283(14) -0.14451(10) 0.0254(3) Uani 1 1 d . . . . .
BR10 Br -0.40281(19) 0.86824(15) -0.35804(10) 0.0258(3) Uani 1 1 d . . . . .
BR11 Br -0.21242(18) 0.69479(15) -0.58989(10) 0.0255(3) Uani 1 1 d . . . . .
BR12 Br -0.41716(18) 0.51295(15) -0.35410(10) 0.0267(3) Uani 1 1 d . . . . .
BR13 Br -0.69833(19) 0.65185(15) -0.56890(10) 0.0267(3) Uani 1 1 d . . . . .
BR14 Br 0.3610(3) 0.00435(18) 0.36300(11) 0.0391(4) Uani 1 1 d . . . . .
PB1 Pb 0.11254(4) 0.97068(4) 0.03771(3) 0.01633(12) Uani 1 1 d . . . . .
PB2 Pb -0.20826(7) 0.85466(5) -0.21546(4) 0.01512(10) Uani 1 1 d . . . . .
PB3 Pb -0.53109(4) 0.75038(4) -0.47569(3) 0.01766(12) 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 N1 1.460(17) . ?
C1 C2 1.51(2) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 C3 1.522(17) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.53(2) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 N2 1.479(15) . ?
C4 C5 1.521(18) . ?
C4 H4 0.9800 . ?
C5 O1 1.20(2) . ?
C5 O2 1.310(19) . ?
C5 H5 0.9800 . ?
C6 N3 1.50(2) . ?
C6 C7 1.505(18) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.51(2) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C9 1.529(19) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 N4 1.493(18) . ?
C9 C10 1.541(17) . ?
C9 H9 0.9800 . ?
C10 O3 1.213(17) . ?
C10 O4 1.296(17) . ?
C10 H10 0.9800 . ?
C11 C12 1.484(17) . ?
C11 N5 1.493(17) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.535(17) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C14 1.514(17) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 N6 1.501(18) . ?
C14 C15 1.513(17) . ?
C14 H14 0.9800 . ?
C15 O5 1.206(18) . ?
C15 O6 1.305(17) . ?
C15 H15 0.9800 . ?
C16 C17 1.49(2) . ?
C16 N7 1.507(17) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.510(17) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C19 1.555(17) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 N8 1.476(16) . ?
C19 C20 1.507(19) . ?
C19 H19 0.9800 . ?
C20 O7 1.219(16) . ?
C20 O8 1.321(17) . ?
C20 H20 0.9800 . ?
N1 H1C 0.8900 . ?
N1 H1D 0.8900 . ?
N1 H1E 0.8900 . ?
N2 H2C 0.8900 . ?
N2 H2D 0.8900 . ?
N2 H2E 0.8900 . ?
N3 H3C 0.8900 . ?
N3 H3D 0.8900 . ?
N3 H3E 0.8900 . ?
N4 H4A 0.8900 . ?
N4 H4B 0.8900 . ?
N4 H4C 0.8900 . ?
N5 H5A 0.8900 . ?
N5 H5B 0.8900 . ?
N5 H5C 0.8900 . ?
N6 H6C 0.8900 . ?
N6 H6D 0.8900 . ?
N6 H6E 0.8900 . ?
N7 H7C 0.8900 . ?
N7 H7D 0.8900 . ?
N7 H7E 0.8900 . ?
N8 H8C 0.8900 . ?
N8 H8D 0.8900 . ?
N8 H8E 0.8900 . ?
O1 H1 0.8200 . ?
O4 H4D 0.8200 . ?
O6 H6 0.8200 . ?
O7 H7 0.8200 . ?
O9 H9A 0.8451 . ?
O9 H9B 0.8497 . ?
O10 H1OA 0.8482 . ?
O10 H10B 0.8524 . ?
BR1 PB1 2.9403(17) . ?
BR2 PB2 3.008(2) 1_655 ?
BR2 PB1 3.2165(19) . ?
BR3 PB1 3.0940(18) . ?
BR4 PB1 2.9064(17) . ?
BR5 PB1 2.9012(18) . ?
BR6 PB2 2.9929(17) . ?
BR6 PB1 3.0512(16) . ?
BR7 PB2 3.041(2) . ?
BR8 PB2 2.884(2) . ?
BR9 PB2 3.059(2) . ?
BR10 PB2 2.9612(18) . ?
BR10 PB3 3.1139(16) . ?
BR11 PB3 2.8795(19) . ?
BR12 PB3 2.8235(19) . ?
BR13 PB3 2.8681(17) . ?
PB2 BR2 3.009(2) 1_455 ?

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
N1 C1 C2 110.6(12) . . ?
N1 C1 H1A 109.5 . . ?
C2 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 108.1 . . ?
C1 C2 C3 111.3(11) . . ?
C1 C2 H2A 109.4 . . ?
C3 C2 H2A 109.4 . . ?
C1 C2 H2B 109.4 . . ?
C3 C2 H2B 109.4 . . ?
H2A C2 H2B 108.0 . . ?
C2 C3 C4 113.1(12) . . ?
C2 C3 H3A 108.9 . . ?
C4 C3 H3A 108.9 . . ?
C2 C3 H3B 108.9 . . ?
C4 C3 H3B 108.9 . . ?
H3A C3 H3B 107.8 . . ?
N2 C4 C5 105.9(11) . . ?
N2 C4 C3 109.5(11) . . ?
C5 C4 C3 110.4(11) . . ?
N2 C4 H4 110.3 . . ?
C5 C4 H4 110.3 . . ?
C3 C4 H4 110.3 . . ?
O1 C5 O2 125.6(14) . . ?
O1 C5 C4 120.7(14) . . ?
O2 C5 C4 113.7(13) . . ?
O1 C5 H5 90.3 . . ?
O2 C5 H5 90.3 . . ?
C4 C5 H5 90.3 . . ?
N3 C6 C7 111.8(13) . . ?
N3 C6 H6A 109.3 . . ?
C7 C6 H6A 109.3 . . ?
N3 C6 H6B 109.3 . . ?
C7 C6 H6B 109.3 . . ?
H6A C6 H6B 107.9 . . ?
C6 C7 C8 111.5(12) . . ?
C6 C7 H7A 109.3 . . ?
C8 C7 H7A 109.3 . . ?
C6 C7 H7B 109.3 . . ?
C8 C7 H7B 109.3 . . ?
H7A C7 H7B 108.0 . . ?
C7 C8 C9 112.4(11) . . ?
C7 C8 H8A 109.1 . . ?
C9 C8 H8A 109.1 . . ?
C7 C8 H8B 109.1 . . ?
C9 C8 H8B 109.1 . . ?
H8A C8 H8B 107.9 . . ?
N4 C9 C8 112.1(11) . . ?
N4 C9 C10 109.2(10) . . ?
C8 C9 C10 113.0(11) . . ?
N4 C9 H9 107.4 . . ?
C8 C9 H9 107.4 . . ?
C10 C9 H9 107.4 . . ?
O3 C10 O4 125.6(12) . . ?
O3 C10 C9 122.5(13) . . ?
O4 C10 C9 111.6(11) . . ?
O3 C10 H10 91.6 . . ?
O4 C10 H10 91.6 . . ?
C9 C10 H10 91.6 . . ?
C12 C11 N5 111.4(10) . . ?
C12 C11 H11A 109.3 . . ?
N5 C11 H11A 109.3 . . ?
C12 C11 H11B 109.3 . . ?
N5 C11 H11B 109.3 . . ?
H11A C11 H11B 108.0 . . ?
C11 C12 C13 109.7(10) . . ?
C11 C12 H12A 109.7 . . ?
C13 C12 H12A 109.7 . . ?
C11 C12 H12B 109.7 . . ?
C13 C12 H12B 109.7 . . ?
H12A C12 H12B 108.2 . . ?
C14 C13 C12 114.0(10) . . ?
C14 C13 H13A 108.7 . . ?
C12 C13 H13A 108.7 . . ?
C14 C13 H13B 108.7 . . ?
C12 C13 H13B 108.7 . . ?
H13A C13 H13B 107.6 . . ?
N6 C14 C15 110.8(11) . . ?
N6 C14 C13 111.9(10) . . ?
C15 C14 C13 113.9(11) . . ?
N6 C14 H14 106.6 . . ?
C15 C14 H14 106.6 . . ?
C13 C14 H14 106.6 . . ?
O5 C15 O6 125.2(12) . . ?
O5 C15 C14 121.6(12) . . ?
O6 C15 C14 113.1(12) . . ?
O5 C15 H15 91.0 . . ?
O6 C15 H15 91.0 . . ?
C14 C15 H15 91.0 . . ?
C17 C16 N7 111.6(11) . . ?
C17 C16 H16A 109.3 . . ?
N7 C16 H16A 109.3 . . ?
C17 C16 H16B 109.3 . . ?
N7 C16 H16B 109.3 . . ?
H16A C16 H16B 108.0 . . ?
C16 C17 C18 109.2(10) . . ?
C16 C17 H17A 109.8 . . ?
C18 C17 H17A 109.8 . . ?
C16 C17 H17B 109.8 . . ?
C18 C17 H17B 109.8 . . ?
H17A C17 H17B 108.3 . . ?
C17 C18 C19 114.9(10) . . ?
C17 C18 H18A 108.5 . . ?
C19 C18 H18A 108.5 . . ?
C17 C18 H18B 108.5 . . ?
C19 C18 H18B 108.5 . . ?
H18A C18 H18B 107.5 . . ?
N8 C19 C20 107.9(10) . . ?
N8 C19 C18 112.5(10) . . ?
C20 C19 C18 109.6(10) . . ?
N8 C19 H19 109.0 . . ?
C20 C19 H19 109.0 . . ?
C18 C19 H19 109.0 . . ?
O7 C20 O8 123.3(13) . . ?
O7 C20 C19 121.3(12) . . ?
O8 C20 C19 115.4(11) . . ?
O7 C20 H20 90.5 . . ?
O8 C20 H20 90.5 . . ?
C19 C20 H20 90.5 . . ?
C1 N1 H1C 109.5 . . ?
C1 N1 H1D 109.5 . . ?
H1C N1 H1D 109.5 . . ?
C1 N1 H1E 109.5 . . ?
H1C N1 H1E 109.5 . . ?
H1D N1 H1E 109.5 . . ?
C4 N2 H2C 109.5 . . ?
C4 N2 H2D 109.5 . . ?
H2C N2 H2D 109.5 . . ?
C4 N2 H2E 109.5 . . ?
H2C N2 H2E 109.5 . . ?
H2D N2 H2E 109.5 . . ?
C6 N3 H3C 109.5 . . ?
C6 N3 H3D 109.5 . . ?
H3C N3 H3D 109.5 . . ?
C6 N3 H3E 109.5 . . ?
H3C N3 H3E 109.5 . . ?
H3D N3 H3E 109.5 . . ?
C9 N4 H4A 109.5 . . ?
C9 N4 H4B 109.5 . . ?
H4A N4 H4B 109.5 . . ?
C9 N4 H4C 109.5 . . ?
H4A N4 H4C 109.5 . . ?
H4B N4 H4C 109.5 . . ?
C11 N5 H5A 109.5 . . ?
C11 N5 H5B 109.5 . . ?
H5A N5 H5B 109.5 . . ?
C11 N5 H5C 109.5 . . ?
H5A N5 H5C 109.5 . . ?
H5B N5 H5C 109.5 . . ?
C14 N6 H6C 109.5 . . ?
C14 N6 H6D 109.5 . . ?
H6C N6 H6D 109.5 . . ?
C14 N6 H6E 109.5 . . ?
H6C N6 H6E 109.5 . . ?
H6D N6 H6E 109.5 . . ?
C16 N7 H7C 109.5 . . ?
C16 N7 H7D 109.5 . . ?
H7C N7 H7D 109.5 . . ?
C16 N7 H7E 109.5 . . ?
H7C N7 H7E 109.5 . . ?
H7D N7 H7E 109.5 . . ?
C19 N8 H8C 109.5 . . ?
C19 N8 H8D 109.5 . . ?
H8C N8 H8D 109.5 . . ?
C19 N8 H8E 109.5 . . ?
H8C N8 H8E 109.5 . . ?
H8D N8 H8E 109.5 . . ?
C5 O1 H1 109.5 . . ?
C10 O4 H4D 109.5 . . ?
C15 O6 H6 109.5 . . ?
C20 O7 H7 109.5 . . ?
H9A O9 H9B 108.2 . . ?
H1OA O10 H10B 107.6 . . ?
PB2 BR2 PB1 172.51(5) 1_655 . ?
PB2 BR6 PB1 153.62(6) . . ?
PB2 BR10 PB3 153.41(6) . . ?
BR5 PB1 BR4 86.55(5) . . ?
BR5 PB1 BR1 88.45(6) . . ?
BR4 PB1 BR1 89.07(6) . . ?
BR5 PB1 BR6 94.70(6) . . ?
BR4 PB1 BR6 85.61(5) . . ?
BR1 PB1 BR6 173.63(5) . . ?
BR5 PB1 BR3 88.56(5) . . ?
BR4 PB1 BR3 174.72(5) . . ?
BR1 PB1 BR3 92.78(6) . . ?
BR6 PB1 BR3 92.82(5) . . ?
BR5 PB1 BR2 171.77(5) . . ?
BR4 PB1 BR2 85.23(5) . . ?
BR1 PB1 BR2 91.12(6) . . ?
BR6 PB1 BR2 84.96(5) . . ?
BR3 PB1 BR2 99.67(5) . . ?
BR8 PB2 BR10 91.57(5) . . ?
BR8 PB2 BR6 87.38(5) . . ?
BR10 PB2 BR6 174.86(5) . . ?
BR8 PB2 BR2 90.88(4) . 1_455 ?
BR10 PB2 BR2 86.33(6) . 1_455 ?
BR6 PB2 BR2 88.65(6) . 1_455 ?
BR8 PB2 BR7 92.59(5) . . ?
BR10 PB2 BR7 93.76(6) . . ?
BR6 PB2 BR7 91.32(6) . . ?
BR2 PB2 BR7 176.53(5) 1_455 . ?
BR8 PB2 BR9 178.40(5) . . ?
BR10 PB2 BR9 88.84(5) . . ?
BR6 PB2 BR9 92.35(5) . . ?
BR2 PB2 BR9 90.70(5) 1_455 . ?
BR7 PB2 BR9 85.84(4) . . ?
BR12 PB3 BR13 92.77(6) . . ?
BR12 PB3 BR11 88.10(5) . . ?
BR13 PB3 BR11 91.99(6) . . ?
BR12 PB3 BR10 88.09(5) . . ?
BR13 PB3 BR10 171.44(4) . . ?
BR11 PB3 BR10 96.55(6) . . ?

_refine_diff_density_max         1.310
_refine_diff_density_min         -1.415
_refine_diff_density_rms         0.180

####################################################################### 
# 
# 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_f
_database_code_depnum_ccdc_archive 'CCDC 1886426'
loop_
_audit_author_name
_audit_author_address
'Maroua Ben Haj Salah'
;University of Angers
France
;
_audit_update_record             
;
2018-12-20 deposited with the CCDC.	2019-03-06 downloaded from the CCDC.
;

_audit_creation_date             2018-08-29T11:56:36-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         '6 (C6 H16 N2 O2), Pb5 Br22, 4 H2 O'
_chemical_formula_sum            'C36 H104 Br22 N12 O16 Pb5'
_chemical_formula_weight         3755.28

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   26.7956(13)
_cell_length_b                   8.1729(3)
_cell_length_c                   22.9805(11)
_cell_angle_alpha                90
_cell_angle_beta                 112.775(6)
_cell_angle_gamma                90
_cell_volume                     4640.3(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    150.01(10)
_cell_measurement_reflns_used    4295
_cell_measurement_theta_min      3.541
_cell_measurement_theta_max      72.411

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.084
_exptl_crystal_size_min          0.062
_exptl_crystal_density_diffrn    2.688
_exptl_crystal_F_000             3424

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    28.828
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.58122
_exptl_absorpt_correction_T_max  1

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      150.00(10)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_monochromator  mirror
_diffrn_detector_area_resol_mean 5.199
_diffrn_measurement_device_type  'SuperNova, Single source at offset, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0635
_diffrn_reflns_av_unetI/netI     0.0937
_diffrn_reflns_number            18103
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         3.578
_diffrn_reflns_theta_max         72.669
_diffrn_reflns_theta_full        71.5
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.97
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.97
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.97
_reflns_Friedel_coverage         0
_reflns_number_total             8948
_reflns_number_gt                6517
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    'DIAMOND 3.2k (Crystal Impact GbR, 2014)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0441P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         8948
_refine_ls_number_parameters     419
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_gt           0.0499
_refine_ls_wR_factor_ref         0.1248
_refine_ls_wR_factor_gt          0.11
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_restrained_S_all      0.986
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         2.326
_refine_diff_density_min         -2.762
_refine_diff_density_rms         0.294

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -4.0753 8.506 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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 0.1515(5) 0.8566(16) 0.9327(6) 0.028(3) Uani 1 1 d . . . . .
H1A H 0.169554 0.890928 0.976281 0.034 Uiso 1 1 calc R U . . .
H1B H 0.16064 0.743022 0.92961 0.034 Uiso 1 1 calc R U . . .
C2 C 0.0898(5) 0.8741(16) 0.9121(6) 0.026(3) Uani 1 1 d . . . . .
H2A H 0.072576 0.852047 0.867212 0.031 Uiso 1 1 calc R U . . .
H2B H 0.077284 0.792338 0.933907 0.031 Uiso 1 1 calc R U . . .
C3 C 0.0722(5) 1.0416(16) 0.9252(6) 0.025(3) Uani 1 1 d . U . . .
H3A H 0.091126 1.124829 0.911574 0.03 Uiso 1 1 calc R U . . .
H3B H 0.08238 1.054044 0.970343 0.03 Uiso 1 1 calc R U . . .
C4 C 0.0109(4) 1.0682(15) 0.8915(5) 0.020(2) Uani 1 1 d . . . . .
H4A H -0.000031 1.04086 0.847174 0.024 Uiso 1 1 calc R U . . .
H4B H -0.007857 0.994792 0.909325 0.024 Uiso 1 1 calc R U . . .
C5 C -0.0060(5) 1.2427(15) 0.8970(5) 0.022(2) Uani 1 1 d . U . . .
H5 H -0.045593 1.247026 0.879986 0.026 Uiso 1 1 calc R U . . .
C6 C 0.0150(5) 1.3037(15) 0.9643(5) 0.021(2) Uani 1 1 d . . . . .
C7 C 0.6952(6) 0.5653(18) 0.2975(6) 0.032(3) Uani 1 1 d . . . . .
C8 C 0.6404(7) 0.6057(17) 0.2454(6) 0.039(4) Uani 1 1 d . . . . .
H8 H 0.642562 0.712386 0.227056 0.047 Uiso 1 1 calc R U . . .
C9 C 0.5972(8) 0.612(3) 0.2727(10) 0.078(8) Uani 1 1 d . U . . .
H9A H 0.604536 0.704437 0.30133 0.093 Uiso 1 1 calc R U . . .
H9B H 0.562392 0.630668 0.2387 0.093 Uiso 1 1 calc R U . . .
C10 C 0.5937(10) 0.459(4) 0.3078(11) 0.087(8) Uani 1 1 d . U . . .
H10A H 0.627143 0.451857 0.344804 0.105 Uiso 0.54(2) 1 calc R U P A 1
H10B H 0.593234 0.36707 0.280994 0.105 Uiso 0.54(2) 1 calc R U P A 1
H10C H 0.625481 0.439242 0.345836 0.105 Uiso 0.46(2) 1 calc R U P A 2
H10D H 0.583394 0.362206 0.281515 0.105 Uiso 0.46(2) 1 calc R U P A 2
C11A C 0.5431(16) 0.432(5) 0.3320(17) 0.056(5) Uani 0.54(2) 1 d . U P A 1
H11A H 0.508347 0.448436 0.297519 0.067 Uiso 0.54(2) 1 calc R U P A 1
H11B H 0.544021 0.321887 0.348534 0.067 Uiso 0.54(2) 1 calc R U P A 1
C11B C 0.5403(19) 0.551(5) 0.3212(19) 0.056(5) Uani 0.46(2) 1 d . . P A 2
H11C H 0.547312 0.665672 0.332916 0.067 Uiso 0.46(2) 1 calc R U P A 2
H11D H 0.506103 0.540561 0.285377 0.067 Uiso 0.46(2) 1 calc R U P A 2
C12A C 0.5520(16) 0.552(5) 0.3806(16) 0.056(5) Uani 0.54(2) 1 d . . P A 1
H12A H 0.552877 0.661215 0.364727 0.067 Uiso 0.54(2) 1 calc R U P A 1
H12B H 0.585639 0.53132 0.416239 0.067 Uiso 0.54(2) 1 calc R U P A 1
C12B C 0.5430(19) 0.452(6) 0.372(2) 0.056(5) Uani 0.46(2) 1 d . . P A 2
H12C H 0.579586 0.450398 0.404052 0.067 Uiso 0.46(2) 1 calc R U P A 2
H12D H 0.532258 0.341055 0.358111 0.067 Uiso 0.46(2) 1 calc R U P A 2
C13 C 0.1517(6) 0.9167(17) 0.6012(6) 0.031(3) Uani 1 1 d . . . . .
C14 C 0.2048(5) 0.8232(17) 0.6373(5) 0.027(3) Uani 1 1 d . . . . .
H14 H 0.202894 0.714079 0.618852 0.032 Uiso 1 1 calc R U . . .
C15 C 0.2538(5) 0.9098(17) 0.6376(6) 0.029(3) Uani 1 1 d . . . . .
H15A H 0.284857 0.868543 0.672925 0.035 Uiso 1 1 calc R U . . .
H15B H 0.250146 1.024858 0.645611 0.035 Uiso 1 1 calc R U . . .
C16 C 0.2662(5) 0.8970(18) 0.5787(6) 0.030(3) Uani 1 1 d . U . . .
H16A H 0.237912 0.951629 0.544051 0.036 Uiso 1 1 calc R U . . .
H16B H 0.266316 0.782614 0.567437 0.036 Uiso 1 1 calc R U . . .
C17 C 0.3207(5) 0.9730(18) 0.5878(6) 0.031(3) Uani 1 1 d . . . . .
H17A H 0.320642 1.086464 0.600128 0.037 Uiso 1 1 calc R U . . .
H17B H 0.348821 0.916891 0.622149 0.037 Uiso 1 1 calc R U . . .
C18 C 0.3345(5) 0.9662(17) 0.5300(6) 0.030(3) Uani 1 1 d . . . . .
H18A H 0.372268 0.995416 0.54202 0.036 Uiso 1 1 calc R U . . .
H18B H 0.32991 0.854818 0.514219 0.036 Uiso 1 1 calc R U . . .
BR1 Br 0.50935(7) 0.9565(3) 0.37694(8) 0.0505(4) Uani 1 1 d . . . . .
BR2 Br 0.43060(6) 0.70657(19) 0.47545(7) 0.0369(3) Uani 1 1 d . . . . .
BR3 Br 0.26916(5) 0.83711(16) 0.35186(6) 0.0260(3) Uani 1 1 d . . . . .
BR4 Br 0.40319(6) 1.21854(18) 0.43367(7) 0.0322(3) Uani 1 1 d . . . . .
BR5 Br 0.29866(6) 0.48377(17) 0.49583(6) 0.0283(3) Uani 1 1 d . . . . .
BR6 Br 0.37874(7) 0.56815(18) 0.28696(6) 0.0359(3) Uani 1 1 d . . . . .
BR7 Br 0.23891(6) 0.35244(19) 0.29664(7) 0.0377(3) Uani 1 1 d . . . . .
BR8 Br 0.13067(6) 0.04316(18) 0.14404(6) 0.0303(3) Uani 1 1 d . . . . .
BR9 Br 0.16343(5) 0.11590(16) 0.41866(6) 0.0249(3) Uani 1 1 d . . . . .
BR10 Br 0.06268(6) 0.26705(19) 0.25583(6) 0.0317(3) Uani 1 1 d . . . . .
BR11 Br 0.10291(6) -0.24463(17) 0.26149(6) 0.0289(3) Uani 1 1 d . . . . .
N1 N 0.1703(4) 0.9609(14) 0.8909(5) 0.026(2) Uani 1 1 d . . . . .
H1C H 0.206285 0.961468 0.905967 0.039 Uiso 1 1 calc R U . . .
H1D H 0.158232 1.062733 0.890083 0.039 Uiso 1 1 calc R U . . .
H1E H 0.157402 0.920118 0.851941 0.039 Uiso 1 1 calc R U . . .
N2 N 0.0137(4) 1.3620(13) 0.8607(4) 0.023(2) Uani 1 1 d . . . . .
H2C H 0.014579 1.462073 0.876346 0.035 Uiso 1 1 calc R U . . .
H2D H -0.008735 1.360812 0.820275 0.035 Uiso 1 1 calc R U . . .
H2E H 0.046719 1.333594 0.864058 0.035 Uiso 1 1 calc R U . . .
N3 N 0.2079(5) 0.8079(15) 0.7033(4) 0.029(2) Uani 1 1 d . . . . .
H3C H 0.178339 0.758027 0.703037 0.044 Uiso 1 1 calc R U . . .
H3D H 0.210346 0.907036 0.720178 0.044 Uiso 1 1 calc R U . . .
H3E H 0.237006 0.749484 0.726001 0.044 Uiso 1 1 calc R U . . .
N4 N 0.3007(5) 1.0767(12) 0.4787(5) 0.025(2) Uani 1 1 d . . . . .
H4C H 0.315054 1.084902 0.449762 0.037 Uiso 1 1 calc R U . . .
H4D H 0.29954 1.175284 0.494607 0.037 Uiso 1 1 calc R U . . .
H4E H 0.26738 1.036371 0.461025 0.037 Uiso 1 1 calc R U . . .
N5 N 0.5029(6) 0.530(2) 0.3995(7) 0.058(4) Uani 1 1 d . . . . .
H5A H 0.472493 0.529808 0.364943 0.07 Uiso 0.54(2) 1 calc R U P A 1
H5B H 0.501908 0.612737 0.42437 0.07 Uiso 0.54(2) 1 calc R U P A 1
H5C H 0.505899 0.436162 0.42003 0.07 Uiso 0.54(2) 1 calc R U P A 1
H5D H 0.469595 0.53209 0.369611 0.07 Uiso 0.46(2) 1 calc R U P A 2
H5E H 0.51332 0.632043 0.412287 0.07 Uiso 0.46(2) 1 calc R U P A 2
H5F H 0.502955 0.471009 0.432013 0.07 Uiso 0.46(2) 1 calc R U P A 2
N6 N 0.6286(5) 0.4773(15) 0.1959(5) 0.036(3) Uani 1 1 d . . . . .
H6A H 0.597016 0.498669 0.164583 0.053 Uiso 1 1 calc R U . . .
H6B H 0.627038 0.380024 0.212449 0.053 Uiso 1 1 calc R U . . .
H6C H 0.654687 0.476612 0.180928 0.053 Uiso 1 1 calc R U . . .
O1 O 0.0508(4) 1.4080(11) 0.9841(4) 0.0250(18) Uani 1 1 d . . . . .
O2 O -0.0085(4) 1.2324(12) 0.9977(4) 0.033(2) Uani 1 1 d . . . . .
H2 H 0.003529 1.26989 1.033637 0.049 Uiso 1 1 calc R U . . .
O3 O 0.7078(5) 0.6805(13) 0.3405(5) 0.044(3) Uani 1 1 d . . . . .
H3 H 0.737003 0.658995 0.368905 0.067 Uiso 1 1 calc R U . . .
O4 O 0.7214(4) 0.4481(13) 0.2977(5) 0.040(2) Uani 1 1 d . . . . .
O5 O 0.1246(5) 0.9713(15) 0.6263(4) 0.042(3) Uani 1 1 d . . . . .
O6 O 0.1403(4) 0.9145(15) 0.5396(4) 0.044(3) Uani 1 1 d . . . . .
H6 H 0.11155 0.962153 0.52099 0.066 Uiso 1 1 calc R U . . .
O7 O 0.1988(5) 0.163(2) 0.0630(5) 0.064(4) Uani 1 1 d . . . . .
O8 O 0.0340(3) 0.1430(10) 0.6114(3) 0.0214(17) Uani 1 1 d . . . . .
PB1 Pb 0.5 1 0.5 0.03070(17) Uani 1 2 d S . P . .
PB2 Pb 0.33380(2) 0.52626(6) 0.38862(2) 0.02039(11) Uani 1 1 d . . . . .
PB3 Pb 0.15548(2) 0.07067(6) 0.27994(2) 0.01992(11) Uani 1 1 d . . . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 N1 1.509(17) . ?
C1 C2 1.539(19) . ?
C1 H1A 0.97 . ?
C1 H1B 0.97 . ?
C2 C3 1.516(17) . ?
C2 H2A 0.97 . ?
C2 H2B 0.97 . ?
C3 C4 1.537(16) . ?
C3 H3A 0.97 . ?
C3 H3B 0.97 . ?
C4 C5 1.516(16) . ?
C4 H4A 0.97 . ?
C4 H4B 0.97 . ?
C5 N2 1.504(15) . ?
C5 C6 1.512(15) . ?
C5 H5 0.98 . ?
C6 O1 1.230(16) . ?
C6 O2 1.304(15) . ?
C7 O4 1.187(18) . ?
C7 O3 1.311(16) . ?
C7 C8 1.53(2) . ?
C8 N6 1.489(17) . ?
C8 C9 1.52(3) . ?
C8 H8 0.98 . ?
C9 C10 1.51(4) . ?
C9 H9A 0.97 . ?
C9 H9B 0.97 . ?
C10 C11A 1.67(4) . ?
C10 C11B 1.75(5) . ?
C10 H10A 0.97 . ?
C10 H10B 0.97 . ?
C10 H10C 0.97 . ?
C10 H10D 0.97 . ?
C11A C12A 1.44(5) . ?
C11A H11A 0.97 . ?
C11A H11B 0.97 . ?
C11B C12B 1.40(6) . ?
C11B H11C 0.97 . ?
C11B H11D 0.97 . ?
C12A N5 1.55(4) . ?
C12A H12A 0.97 . ?
C12A H12B 0.97 . ?
C12B N5 1.58(5) . ?
C12B H12C 0.97 . ?
C12B H12D 0.97 . ?
C13 O5 1.174(18) . ?
C13 O6 1.327(15) . ?
C13 C14 1.544(19) . ?
C14 C15 1.488(17) . ?
C14 N3 1.492(15) . ?
C14 H14 0.98 . ?
C15 C16 1.519(18) . ?
C15 H15A 0.97 . ?
C15 H15B 0.97 . ?
C16 C17 1.524(19) . ?
C16 H16A 0.97 . ?
C16 H16B 0.97 . ?
C17 C18 1.511(19) . ?
C17 H17A 0.97 . ?
C17 H17B 0.97 . ?
C18 N4 1.483(17) . ?
C18 H18A 0.97 . ?
C18 H18B 0.97 . ?
BR1 PB1 2.9555(18) . ?
BR2 PB1 2.9521(14) . ?
BR2 PB2 2.9790(15) . ?
BR3 PB2 3.0059(14) . ?
BR4 PB1 3.0301(14) . ?
BR4 PB2 3.0600(15) 1_565 ?
BR5 PB2 2.9788(14) . ?
BR6 PB2 3.0336(15) . ?
BR7 PB2 2.9647(14) . ?
BR7 PB3 3.1280(15) . ?
BR8 PB3 2.9390(13) . ?
BR9 PB3 3.1336(13) . ?
BR10 PB3 2.8284(15) . ?
BR11 PB3 2.8882(14) . ?
N1 H1C 0.89 . ?
N1 H1D 0.89 . ?
N1 H1E 0.89 . ?
N2 H2C 0.89 . ?
N2 H2D 0.89 . ?
N2 H2E 0.89 . ?
N3 H3C 0.89 . ?
N3 H3D 0.89 . ?
N3 H3E 0.89 . ?
N4 H4C 0.89 . ?
N4 H4D 0.89 . ?
N4 H4E 0.89 . ?
N5 H5A 0.89 . ?
N5 H5B 0.89 . ?
N5 H5C 0.89 . ?
N5 H5D 0.89 . ?
N5 H5E 0.89 . ?
N5 H5F 0.89 . ?
N6 H6A 0.89 . ?
N6 H6B 0.89 . ?
N6 H6C 0.89 . ?
O2 H2 0.82 . ?
O3 H3 0.82 . ?
O6 H6 0.82 . ?
PB1 BR2 2.9522(15) 3_676 ?
PB1 BR1 2.9556(18) 3_676 ?
PB1 BR4 3.0301(14) 3_676 ?
PB2 BR4 3.0600(15) 1_545 ?

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
N1 C1 C2 109.6(10) . . ?
N1 C1 H1A 109.8 . . ?
C2 C1 H1A 109.8 . . ?
N1 C1 H1B 109.8 . . ?
C2 C1 H1B 109.8 . . ?
H1A C1 H1B 108.2 . . ?
C3 C2 C1 113.7(11) . . ?
C3 C2 H2A 108.8 . . ?
C1 C2 H2A 108.8 . . ?
C3 C2 H2B 108.8 . . ?
C1 C2 H2B 108.8 . . ?
H2A C2 H2B 107.7 . . ?
C2 C3 C4 112.4(11) . . ?
C2 C3 H3A 109.1 . . ?
C4 C3 H3A 109.1 . . ?
C2 C3 H3B 109.1 . . ?
C4 C3 H3B 109.1 . . ?
H3A C3 H3B 107.8 . . ?
C5 C4 C3 112.7(10) . . ?
C5 C4 H4A 109.1 . . ?
C3 C4 H4A 109.1 . . ?
C5 C4 H4B 109.1 . . ?
C3 C4 H4B 109.1 . . ?
H4A C4 H4B 107.8 . . ?
N2 C5 C6 106.4(9) . . ?
N2 C5 C4 112.6(9) . . ?
C6 C5 C4 113.1(10) . . ?
N2 C5 H5 108.2 . . ?
C6 C5 H5 108.2 . . ?
C4 C5 H5 108.2 . . ?
O1 C6 O2 125.2(11) . . ?
O1 C6 C5 122.3(11) . . ?
O2 C6 C5 112.5(11) . . ?
O4 C7 O3 126.8(13) . . ?
O4 C7 C8 124.3(12) . . ?
O3 C7 C8 108.9(13) . . ?
N6 C8 C9 111.8(14) . . ?
N6 C8 C7 107.6(12) . . ?
C9 C8 C7 109.8(13) . . ?
N6 C8 H8 109.2 . . ?
C9 C8 H8 109.2 . . ?
C7 C8 H8 109.2 . . ?
C10 C9 C8 114.1(16) . . ?
C10 C9 H9A 108.7 . . ?
C8 C9 H9A 108.7 . . ?
C10 C9 H9B 108.7 . . ?
C8 C9 H9B 108.7 . . ?
H9A C9 H9B 107.6 . . ?
C9 C10 C11A 121(2) . . ?
C9 C10 C11B 88(2) . . ?
C9 C10 H10A 107 . . ?
C11A C10 H10A 107 . . ?
C9 C10 H10B 107 . . ?
C11A C10 H10B 107 . . ?
H10A C10 H10B 106.8 . . ?
C9 C10 H10C 114 . . ?
C11B C10 H10C 114 . . ?
C9 C10 H10D 114 . . ?
C11B C10 H10D 114 . . ?
H10C C10 H10D 111.2 . . ?
C12A C11A C10 105(3) . . ?
C12A C11A H11A 110.8 . . ?
C10 C11A H11A 110.8 . . ?
C12A C11A H11B 110.8 . . ?
C10 C11A H11B 110.8 . . ?
H11A C11A H11B 108.9 . . ?
C12B C11B C10 97(3) . . ?
C12B C11B H11C 112.4 . . ?
C10 C11B H11C 112.4 . . ?
C12B C11B H11D 112.4 . . ?
C10 C11B H11D 112.4 . . ?
H11C C11B H11D 110 . . ?
C11A C12A N5 104(3) . . ?
C11A C12A H12A 111 . . ?
N5 C12A H12A 111 . . ?
C11A C12A H12B 111 . . ?
N5 C12A H12B 111 . . ?
H12A C12A H12B 109 . . ?
C11B C12B N5 106(3) . . ?
C11B C12B H12C 110.5 . . ?
N5 C12B H12C 110.5 . . ?
C11B C12B H12D 110.5 . . ?
N5 C12B H12D 110.5 . . ?
H12C C12B H12D 108.7 . . ?
O5 C13 O6 126.6(14) . . ?
O5 C13 C14 122.8(11) . . ?
O6 C13 C14 110.4(12) . . ?
C15 C14 N3 109.4(11) . . ?
C15 C14 C13 113.3(11) . . ?
N3 C14 C13 105.3(10) . . ?
C15 C14 H14 109.6 . . ?
N3 C14 H14 109.6 . . ?
C13 C14 H14 109.6 . . ?
C14 C15 C16 117.3(12) . . ?
C14 C15 H15A 108 . . ?
C16 C15 H15A 108 . . ?
C14 C15 H15B 108 . . ?
C16 C15 H15B 108 . . ?
H15A C15 H15B 107.2 . . ?
C15 C16 C17 112.2(11) . . ?
C15 C16 H16A 109.2 . . ?
C17 C16 H16A 109.2 . . ?
C15 C16 H16B 109.2 . . ?
C17 C16 H16B 109.2 . . ?
H16A C16 H16B 107.9 . . ?
C18 C17 C16 114.3(11) . . ?
C18 C17 H17A 108.7 . . ?
C16 C17 H17A 108.7 . . ?
C18 C17 H17B 108.7 . . ?
C16 C17 H17B 108.7 . . ?
H17A C17 H17B 107.6 . . ?
N4 C18 C17 113.2(11) . . ?
N4 C18 H18A 108.9 . . ?
C17 C18 H18A 108.9 . . ?
N4 C18 H18B 108.9 . . ?
C17 C18 H18B 108.9 . . ?
H18A C18 H18B 107.7 . . ?
PB1 BR2 PB2 148.28(6) . . ?
PB1 BR4 PB2 160.80(6) . 1_565 ?
PB2 BR7 PB3 144.61(5) . . ?
C1 N1 H1C 109.5 . . ?
C1 N1 H1D 109.5 . . ?
H1C N1 H1D 109.5 . . ?
C1 N1 H1E 109.5 . . ?
H1C N1 H1E 109.5 . . ?
H1D N1 H1E 109.5 . . ?
C5 N2 H2C 109.5 . . ?
C5 N2 H2D 109.5 . . ?
H2C N2 H2D 109.5 . . ?
C5 N2 H2E 109.5 . . ?
H2C N2 H2E 109.5 . . ?
H2D N2 H2E 109.5 . . ?
C14 N3 H3C 109.5 . . ?
C14 N3 H3D 109.5 . . ?
H3C N3 H3D 109.5 . . ?
C14 N3 H3E 109.5 . . ?
H3C N3 H3E 109.5 . . ?
H3D N3 H3E 109.5 . . ?
C18 N4 H4C 109.5 . . ?
C18 N4 H4D 109.5 . . ?
H4C N4 H4D 109.5 . . ?
C18 N4 H4E 109.5 . . ?
H4C N4 H4E 109.5 . . ?
H4D N4 H4E 109.5 . . ?
C12A N5 H5A 109.5 . . ?
C12A N5 H5B 109.5 . . ?
H5A N5 H5B 109.5 . . ?
C12A N5 H5C 109.5 . . ?
H5A N5 H5C 109.5 . . ?
H5B N5 H5C 109.5 . . ?
C12B N5 H5D 109.5 . . ?
C12B N5 H5E 109.5 . . ?
H5D N5 H5E 109.5 . . ?
C12B N5 H5F 109.5 . . ?
H5D N5 H5F 109.5 . . ?
H5E N5 H5F 109.5 . . ?
C8 N6 H6A 109.5 . . ?
C8 N6 H6B 109.5 . . ?
H6A N6 H6B 109.5 . . ?
C8 N6 H6C 109.5 . . ?
H6A N6 H6C 109.5 . . ?
H6B N6 H6C 109.5 . . ?
C6 O2 H2 109.5 . . ?
C7 O3 H3 109.5 . . ?
C13 O6 H6 109.5 . . ?
BR2 PB1 BR2 180 . 3_676 ?
BR2 PB1 BR1 90.00(5) . . ?
BR2 PB1 BR1 90.00(5) 3_676 . ?
BR2 PB1 BR1 90.00(5) . 3_676 ?
BR2 PB1 BR1 90.00(5) 3_676 3_676 ?
BR1 PB1 BR1 180 . 3_676 ?
BR2 PB1 BR4 88.31(4) . 3_676 ?
BR2 PB1 BR4 91.69(4) 3_676 3_676 ?
BR1 PB1 BR4 92.14(5) . 3_676 ?
BR1 PB1 BR4 87.86(5) 3_676 3_676 ?
BR2 PB1 BR4 91.69(4) . . ?
BR2 PB1 BR4 88.31(4) 3_676 . ?
BR1 PB1 BR4 87.86(5) . . ?
BR1 PB1 BR4 92.14(5) 3_676 . ?
BR4 PB1 BR4 180 3_676 . ?
BR7 PB2 BR5 94.33(4) . . ?
BR7 PB2 BR2 177.02(5) . . ?
BR5 PB2 BR2 88.61(4) . . ?
BR7 PB2 BR3 87.87(4) . . ?
BR5 PB2 BR3 89.93(4) . . ?
BR2 PB2 BR3 91.59(4) . . ?
BR7 PB2 BR6 89.52(5) . . ?
BR5 PB2 BR6 175.48(4) . . ?
BR2 PB2 BR6 87.58(4) . . ?
BR3 PB2 BR6 92.61(4) . . ?
BR7 PB2 BR4 95.08(5) . 1_545 ?
BR5 PB2 BR4 88.26(4) . 1_545 ?
BR2 PB2 BR4 85.55(4) . 1_545 ?
BR3 PB2 BR4 176.65(4) . 1_545 ?
BR6 PB2 BR4 89.02(4) . 1_545 ?
BR10 PB3 BR11 97.80(5) . . ?
BR10 PB3 BR8 90.87(4) . . ?
BR11 PB3 BR8 83.04(4) . . ?
BR10 PB3 BR7 97.97(5) . . ?
BR11 PB3 BR7 163.67(5) . . ?
BR8 PB3 BR7 92.50(4) . . ?
BR10 PB3 BR9 80.83(4) . . ?
BR11 PB3 BR9 95.27(4) . . ?
BR8 PB3 BR9 171.25(4) . . ?
BR7 PB3 BR9 91.40(4) . . ?

####################################################################### 
# 
# 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_l-lysine-fi
_database_code_depnum_ccdc_archive 'CCDC 1886425'
loop_
_audit_author_name
_audit_author_address
'Maroua Ben Haj Salah'
;University of Angers
France
;
_audit_update_record             
;
2018-12-20 deposited with the CCDC.	2019-03-06 downloaded from the CCDC.
;

_audit_creation_date             2018-07-11T10:37:08-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         '3(C6 H16 N2 O2), Pb2 Br9, Br, H2 O'
_chemical_formula_sum            'C18 H50 Br10 N6 O7 Pb2'
_chemical_formula_weight         1676.12
_chemical_absolute_configuration rmad

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_Int_Tables_number      4
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   12.3316(4)
_cell_length_b                   8.0863(2)
_cell_length_c                   23.0098(7)
_cell_angle_alpha                90
_cell_angle_beta                 101.621(3)
_cell_angle_gamma                90
_cell_volume                     2247.44(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    150.0(1)
_cell_measurement_reflns_used    5422
_cell_measurement_theta_min      3.614
_cell_measurement_theta_max      72.144

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.243
_exptl_crystal_size_mid          0.097
_exptl_crystal_size_min          0.042
_exptl_crystal_density_diffrn    2.477
_exptl_crystal_F_000             1540

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    25.132
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.58612
_exptl_absorpt_correction_T_max  1

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      150.0(1)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_monochromator  mirror
_diffrn_detector_area_resol_mean 5.199
_diffrn_measurement_device_type  'SuperNova, Single source at offset, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0483
_diffrn_reflns_av_unetI/netI     0.0584
_diffrn_reflns_number            9202
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         3.788
_diffrn_reflns_theta_max         72.403
_diffrn_reflns_theta_full        70
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.972
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_point_group_measured_fraction_full 0.665
_diffrn_reflns_point_group_measured_fraction_max 0.648
_reflns_Friedel_fraction_full    0.283
_reflns_Friedel_fraction_max     0.271
_reflns_Friedel_coverage         0.239
_reflns_number_total             5750
_reflns_number_gt                5471
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    'DIAMOND 3.2k (Crystal Impact GbR, 2014)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1311P)²+8.7806P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         5750
_refine_ls_number_parameters     418
_refine_ls_number_restraints     33
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0599
_refine_ls_wR_factor_ref         0.1686
_refine_ls_wR_factor_gt          0.1649
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_restrained_S_all      1.004
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_abs_structure_details 
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.027(14)
_refine_diff_density_max         3.787
_refine_diff_density_min         -3.426
_refine_diff_density_rms         0.348

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -4.0753 8.506 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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 0.8146(18) 1.048(3) 0.4041(9) 0.036(5) Uani 1 1 d . . . . .
C2 C 0.7732(14) 0.978(3) 0.3428(8) 0.030(4) Uani 1 1 d . . . . .
H2 H 0.795148 0.861656 0.341341 0.036 Uiso 1 1 calc R U . . .
C3 C 0.8253(17) 1.081(3) 0.2997(9) 0.035(5) Uani 1 1 d . . . . .
H3D H 0.794284 1.19162 0.298102 0.042 Uiso 1 1 calc R U . . .
H3E H 0.904035 1.090509 0.315804 0.042 Uiso 1 1 calc R U . . .
C4 C 0.8101(17) 1.015(3) 0.2366(9) 0.034(5) Uani 1 1 d . . . . .
H4A H 0.731906 1.013268 0.218469 0.041 Uiso 1 1 calc R U . . .
H4B H 0.838217 0.903227 0.237212 0.041 Uiso 1 1 calc R U . . .
C5 C 0.8719(13) 1.126(4) 0.2001(8) 0.032(4) Uani 1 1 d . . . . .
H5D H 0.950975 1.117115 0.215269 0.039 Uiso 1 1 calc R U . . .
H5E H 0.850149 1.23992 0.203306 0.039 Uiso 1 1 calc R U . . .
C6 C 0.845(2) 1.071(3) 0.1343(11) 0.046(6) Uani 1 1 d . . . . .
H6D H 0.860514 0.954222 0.131235 0.056 Uiso 1 1 calc R U . . .
H6E H 0.766576 1.088699 0.117937 0.056 Uiso 1 1 calc R U . . .
C7 C 0.621(2) 0.599(4) 0.2273(11) 0.048(7) Uani 1 1 d . . . . .
C8 C 0.5265(19) 0.555(3) 0.1761(9) 0.032(4) Uani 1 1 d . . . . .
H8 H 0.489293 0.455692 0.18664 0.038 Uiso 1 1 calc R U . . .
C9 C 0.564(2) 0.523(3) 0.1165(11) 0.045(6) Uani 1 1 d . . . . .
H9A H 0.617436 0.432955 0.122113 0.054 Uiso 1 1 calc R U . . .
H9B H 0.500799 0.488052 0.086965 0.054 Uiso 1 1 calc R U . . .
C10 C 0.617(3) 0.673(5) 0.0928(14) 0.079(13) Uani 1 1 d . U . . .
H10A H 0.653942 0.734286 0.12744 0.095 Uiso 0.55(3) 1 calc R U P A 1
H10B H 0.555644 0.74228 0.073508 0.095 Uiso 0.55(3) 1 calc R U P A 1
H10C H 0.690078 0.69696 0.115856 0.095 Uiso 0.45(3) 1 calc R U P A 2
H10D H 0.570644 0.771118 0.091083 0.095 Uiso 0.45(3) 1 calc R U P A 2
C11A C 0.699(3) 0.669(5) 0.0502(15) 0.029(6) Uani 0.55(3) 1 d . . P A 1
H11A H 0.744312 0.767579 0.054668 0.034 Uiso 0.55(3) 1 calc R U P A 1
H11B H 0.746868 0.572881 0.05829 0.034 Uiso 0.55(3) 1 calc R U P A 1
C11B C 0.622(3) 0.601(6) 0.0242(19) 0.029(6) Uani 0.45(3) 1 d . . P A 2
H11C H 0.648717 0.487993 0.026379 0.034 Uiso 0.45(3) 1 calc R U P A 2
H11D H 0.548697 0.603852 -0.001343 0.034 Uiso 0.45(3) 1 calc R U P A 2
C12A C 0.631(3) 0.659(5) -0.0093(13) 0.028(6) Uani 0.55(3) 1 d D U P A 1
H12A H 0.589039 0.760803 -0.018089 0.034 Uiso 0.55(3) 1 calc R U P A 1
H12B H 0.579391 0.568332 -0.011476 0.034 Uiso 0.55(3) 1 calc R U P A 1
C12B C 0.694(4) 0.707(6) 0.0029(13) 0.028(6) Uani 0.45(3) 1 d D . P A 2
H12C H 0.765986 0.709445 0.029671 0.034 Uiso 0.45(3) 1 calc R U P A 2
H12D H 0.664896 0.818056 -0.002144 0.034 Uiso 0.45(3) 1 calc R U P A 2
C13 C -0.0123(19) 0.571(3) 0.3295(11) 0.041(6) Uani 1 1 d . . . . .
C14 C 0.098(2) 0.546(3) 0.3138(10) 0.036(5) Uani 1 1 d . . . . .
H14 H 0.095005 0.442992 0.291102 0.043 Uiso 1 1 calc R U . . .
C15 C 0.1988(16) 0.532(3) 0.3677(9) 0.031(5) Uani 1 1 d . . . . .
H15A H 0.185839 0.440994 0.392686 0.038 Uiso 1 1 calc R U . . .
H15B H 0.265227 0.507604 0.352763 0.038 Uiso 1 1 calc R U . . .
C16 C 0.2181(17) 0.687(3) 0.4047(9) 0.033(4) Uani 1 1 d . U . . .
H16A H 0.155825 0.704722 0.423839 0.04 Uiso 1 1 calc R U . . .
H16B H 0.222585 0.781167 0.37909 0.04 Uiso 1 1 calc R U . . .
C17 C 0.3246(16) 0.676(3) 0.4519(8) 0.032(4) Uani 1 1 d . . . . .
H17A H 0.385142 0.644357 0.433144 0.039 Uiso 1 1 calc R U . . .
H17B H 0.316207 0.590994 0.480304 0.039 Uiso 1 1 calc R U . . .
C18 C 0.354(2) 0.842(4) 0.4852(9) 0.043(6) Uani 1 1 d . . . . .
H18A H 0.290296 0.878645 0.500559 0.051 Uiso 1 1 calc R U . . .
H18B H 0.414105 0.822613 0.518739 0.051 Uiso 1 1 calc R U . . .
N1 N 0.6493(13) 0.993(3) 0.3291(8) 0.036(4) Uani 1 1 d . . . . .
H1A H 0.630241 1.097499 0.333683 0.054 Uiso 1 1 calc R U . . .
H1B H 0.620867 0.92853 0.353629 0.054 Uiso 1 1 calc R U . . .
H1C H 0.623241 0.961475 0.291806 0.054 Uiso 1 1 calc R U . . .
N2 N 0.9127(16) 1.170(2) 0.1013(7) 0.036(4) Uani 1 1 d . . . . .
H2A H 0.92333 1.27012 0.11719 0.053 Uiso 1 1 calc R U . . .
H2B H 0.878164 1.177998 0.063536 0.053 Uiso 1 1 calc R U . . .
H2C H 0.97786 1.120176 0.103242 0.053 Uiso 1 1 calc R U . . .
N3 N 0.4455(12) 0.698(2) 0.1690(7) 0.025(3) Uani 1 1 d . . . . .
H3A H 0.481122 0.791504 0.165177 0.038 Uiso 1 1 calc R U . . .
H3B H 0.414879 0.703596 0.200757 0.038 Uiso 1 1 calc R U . . .
H3C H 0.392987 0.681589 0.136768 0.038 Uiso 1 1 calc R U . . .
N4 N 0.7033(19) 0.634(3) -0.0543(7) 0.049(5) Uani 1 1 d D . . . .
H4C H 0.661178 0.605974 -0.089023 0.058 Uiso 0.55(3) 1 calc R U P A 1
H4D H 0.752128 0.554486 -0.042019 0.058 Uiso 0.55(3) 1 calc R U P A 1
H4E H 0.738952 0.727884 -0.058553 0.058 Uiso 0.55(3) 1 calc R U P A 1
H4F H 0.774299 0.61981 -0.055557 0.058 Uiso 0.45(3) 1 calc R U P A 2
H4G H 0.672297 0.702115 -0.083474 0.058 Uiso 0.45(3) 1 calc R U P A 2
H4H H 0.668555 0.537303 -0.058758 0.058 Uiso 0.45(3) 1 calc R U P A 2
N5 N 0.1189(14) 0.680(3) 0.2751(7) 0.034(4) Uani 1 1 d . . . . .
H5A H 0.108291 0.77648 0.291622 0.05 Uiso 1 1 calc R U . . .
H5B H 0.072627 0.670993 0.240182 0.05 Uiso 1 1 calc R U . . .
H5C H 0.188365 0.673817 0.269919 0.05 Uiso 1 1 calc R U . . .
N6 N 0.3865(14) 0.974(3) 0.4477(7) 0.038(5) Uani 1 1 d . . . . .
H6A H 0.457567 0.962233 0.446094 0.057 Uiso 1 1 calc R U . . .
H6B H 0.376105 1.072043 0.463216 0.057 Uiso 1 1 calc R U . . .
H6C H 0.345343 0.966981 0.411258 0.057 Uiso 1 1 calc R U . . .
O1 O 0.9118(15) 0.981(3) 0.4307(9) 0.060(6) Uani 1 1 d . . . . .
H1 H 0.925654 0.900918 0.411469 0.09 Uiso 1 1 calc R U . . .
O2 O 0.7749(17) 1.167(2) 0.4232(8) 0.051(5) Uani 1 1 d . . . . .
O3 O 0.676(3) 0.461(4) 0.2465(13) 0.138(15) Uani 1 1 d . U . . .
H3 H 0.688049 0.458718 0.282872 0.207 Uiso 1 1 calc R U . . .
O4 O 0.6342(13) 0.730(2) 0.2480(7) 0.042(4) Uani 1 1 d . . . . .
O5 O -0.0386(11) 0.468(2) 0.3674(7) 0.040(4) Uani 1 1 d . . . . .
H5 H -0.008347 0.378516 0.364569 0.06 Uiso 1 1 calc R U . . .
O6A O -0.053(3) 0.714(5) 0.3285(16) 0.042(6) Uani 0.52(3) 1 d . U P . .
O6B O -0.091(3) 0.659(5) 0.2933(15) 0.042(6) Uani 0.48(3) 1 d . . P . .
O7 O 0.7488(12) 0.493(2) 0.3734(7) 0.038(4) Uani 1 1 d G . . . .
H7A H 0.747333 0.572033 0.39755 0.058 Uiso 1 1 d G U . . .
H7B H 0.815349 0.474756 0.370315 0.058 Uiso 1 1 d G U . . .
BR1 Br 0.47539(19) 0.2788(4) 0.35392(11) 0.0441(6) Uani 1 1 d . . . . .
BR2 Br 0.23812(16) 0.4416(3) 0.17903(9) 0.0287(4) Uani 1 1 d . . . . .
BR3 Br 0.49635(16) 0.0989(3) 0.17231(9) 0.0309(5) Uani 1 1 d . . . . .
BR4 Br 0.39368(16) -0.1984(3) 0.30027(8) 0.0268(4) Uani 1 1 d . . . . .
BR5 Br 0.15347(18) 0.0935(3) 0.32681(10) 0.0335(5) Uani 1 1 d . . . . .
BR6 Br 0.15225(18) 0.9527(3) 0.15525(9) 0.0341(5) Uani 1 1 d . . . . .
BR7A Br -0.0767(4) 0.5628(9) 0.1680(9) 0.029(3) Uani 0.52(4) 1 d . . P . .
BR7B Br -0.0839(6) 0.5808(9) 0.1392(11) 0.031(3) Uani 0.48(4) 1 d . . P . .
BR8 Br -0.0489(2) 0.8511(3) -0.00656(10) 0.0459(6) Uani 1 1 d . . . . .
BR9 Br 0.2914(3) 0.7056(4) 0.02706(11) 0.0526(7) Uani 1 1 d . . . . .
BR10 Br 0.63690(18) 0.7706(3) 0.45122(9) 0.0367(5) Uani 1 1 d . . . . .
PB1 Pb 0.32560(5) 0.12615(9) 0.25744(3) 0.0218(2) Uani 1 1 d . . . . .
PB2 Pb 0.09631(6) 0.64309(11) 0.08887(3) 0.0330(2) Uani 1 1 d . . . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 O2 1.20(3) . ?
C1 O1 1.35(3) . ?
C1 C2 1.51(3) . ?
C2 N1 1.50(2) . ?
C2 C3 1.53(3) . ?
C2 H2 0.98 . ?
C3 C4 1.52(3) . ?
C3 H3D 0.97 . ?
C3 H3E 0.97 . ?
C4 C5 1.53(3) . ?
C4 H4A 0.97 . ?
C4 H4B 0.97 . ?
C5 C6 1.55(3) . ?
C5 H5D 0.97 . ?
C5 H5E 0.97 . ?
C6 N2 1.48(3) . ?
C6 H6D 0.97 . ?
C6 H6E 0.97 . ?
C7 O4 1.16(4) . ?
C7 O3 1.33(4) . ?
C7 C8 1.52(3) . ?
C8 N3 1.51(3) . ?
C8 C9 1.56(3) . ?
C8 H8 0.98 . ?
C9 C10 1.53(4) . ?
C9 H9A 0.97 . ?
C9 H9B 0.97 . ?
C10 C11A 1.54(4) . ?
C10 C11B 1.70(5) . ?
C10 H10A 0.97 . ?
C10 H10B 0.97 . ?
C10 H10C 0.97 . ?
C10 H10D 0.97 . ?
C11A C12A 1.45(5) . ?
C11A H11A 0.97 . ?
C11A H11B 0.97 . ?
C11B C12B 1.40(7) . ?
C11B H11C 0.97 . ?
C11B H11D 0.97 . ?
C12A N4 1.51(2) . ?
C12A H12A 0.97 . ?
C12A H12B 0.97 . ?
C12B N4 1.46(2) . ?
C12B H12C 0.97 . ?
C12B H12D 0.97 . ?
C13 O6A 1.26(4) . ?
C13 O5 1.29(3) . ?
C13 O6B 1.35(4) . ?
C13 C14 1.49(3) . ?
C14 N5 1.45(3) . ?
C14 C15 1.57(3) . ?
C14 H14 0.98 . ?
C15 C16 1.51(3) . ?
C15 H15A 0.97 . ?
C15 H15B 0.97 . ?
C16 C17 1.53(3) . ?
C16 H16A 0.97 . ?
C16 H16B 0.97 . ?
C17 C18 1.55(4) . ?
C17 H17A 0.97 . ?
C17 H17B 0.97 . ?
C18 N6 1.48(3) . ?
C18 H18A 0.97 . ?
C18 H18B 0.97 . ?
N1 H1A 0.89 . ?
N1 H1B 0.89 . ?
N1 H1C 0.89 . ?
N2 H2A 0.89 . ?
N2 H2B 0.89 . ?
N2 H2C 0.89 . ?
N3 H3A 0.89 . ?
N3 H3B 0.89 . ?
N3 H3C 0.89 . ?
N4 H4C 0.89 . ?
N4 H4D 0.89 . ?
N4 H4E 0.89 . ?
N4 H4F 0.89 . ?
N4 H4G 0.89 . ?
N4 H4H 0.89 . ?
N5 H5A 0.89 . ?
N5 H5B 0.89 . ?
N5 H5C 0.89 . ?
N6 H6A 0.89 . ?
N6 H6B 0.89 . ?
N6 H6C 0.89 . ?
O1 H1 0.82 . ?
O3 H3 0.82 . ?
O5 H5 0.82 . ?
O6A O6B 0.96(5) . ?
O7 H7A 0.8501 . ?
O7 H7B 0.8501 . ?
BR1 PB1 2.866(2) . ?
BR2 PB2 2.925(2) . ?
BR2 PB1 3.184(2) . ?
BR3 PB1 3.159(2) . ?
BR4 PB1 2.869(2) . ?
BR5 PB1 2.9135(19) . ?
BR6 PB2 2.941(2) . ?
BR6 PB1 3.169(2) 1_565 ?
BR7A BR7B 0.666(6) . ?
BR7A PB2 3.139(16) . ?
BR7B PB2 2.752(12) . ?
BR8 PB2 3.010(3) 2 ?
BR8 PB2 3.045(2) . ?
BR9 PB2 3.073(4) . ?
PB1 BR6 3.169(2) 1_545 ?
PB2 BR8 3.010(3) 2_545 ?

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
O2 C1 O1 123(2) . . ?
O2 C1 C2 124(2) . . ?
O1 C1 C2 112(2) . . ?
N1 C2 C1 107.7(16) . . ?
N1 C2 C3 111.2(18) . . ?
C1 C2 C3 107.1(19) . . ?
N1 C2 H2 110.3 . . ?
C1 C2 H2 110.3 . . ?
C3 C2 H2 110.3 . . ?
C4 C3 C2 116(2) . . ?
C4 C3 H3D 108.3 . . ?
C2 C3 H3D 108.3 . . ?
C4 C3 H3E 108.3 . . ?
C2 C3 H3E 108.3 . . ?
H3D C3 H3E 107.4 . . ?
C3 C4 C5 110(2) . . ?
C3 C4 H4A 109.7 . . ?
C5 C4 H4A 109.7 . . ?
C3 C4 H4B 109.7 . . ?
C5 C4 H4B 109.7 . . ?
H4A C4 H4B 108.2 . . ?
C4 C5 C6 109.6(19) . . ?
C4 C5 H5D 109.7 . . ?
C6 C5 H5D 109.7 . . ?
C4 C5 H5E 109.7 . . ?
C6 C5 H5E 109.7 . . ?
H5D C5 H5E 108.2 . . ?
N2 C6 C5 108.4(19) . . ?
N2 C6 H6D 110 . . ?
C5 C6 H6D 110 . . ?
N2 C6 H6E 110 . . ?
C5 C6 H6E 110 . . ?
H6D C6 H6E 108.4 . . ?
O4 C7 O3 127(2) . . ?
O4 C7 C8 124(3) . . ?
O3 C7 C8 109(3) . . ?
N3 C8 C7 106.9(18) . . ?
N3 C8 C9 109.9(17) . . ?
C7 C8 C9 114(2) . . ?
N3 C8 H8 108.7 . . ?
C7 C8 H8 108.7 . . ?
C9 C8 H8 108.7 . . ?
C10 C9 C8 114(2) . . ?
C10 C9 H9A 108.8 . . ?
C8 C9 H9A 108.8 . . ?
C10 C9 H9B 108.8 . . ?
C8 C9 H9B 108.8 . . ?
H9A C9 H9B 107.7 . . ?
C9 C10 C11A 126(3) . . ?
C9 C10 C11B 99(3) . . ?
C9 C10 H10A 105.9 . . ?
C11A C10 H10A 105.9 . . ?
C9 C10 H10B 105.9 . . ?
C11A C10 H10B 105.9 . . ?
H10A C10 H10B 106.2 . . ?
C9 C10 H10C 112 . . ?
C11B C10 H10C 112 . . ?
C9 C10 H10D 112 . . ?
C11B C10 H10D 112 . . ?
H10C C10 H10D 109.7 . . ?
C12A C11A C10 106(3) . . ?
C12A C11A H11A 110.6 . . ?
C10 C11A H11A 110.6 . . ?
C12A C11A H11B 110.6 . . ?
C10 C11A H11B 110.6 . . ?
H11A C11A H11B 108.7 . . ?
C12B C11B C10 105(3) . . ?
C12B C11B H11C 110.7 . . ?
C10 C11B H11C 110.7 . . ?
C12B C11B H11D 110.7 . . ?
C10 C11B H11D 110.7 . . ?
H11C C11B H11D 108.8 . . ?
C11A C12A N4 110(2) . . ?
C11A C12A H12A 109.6 . . ?
N4 C12A H12A 109.6 . . ?
C11A C12A H12B 109.6 . . ?
N4 C12A H12B 109.6 . . ?
H12A C12A H12B 108.1 . . ?
C11B C12B N4 104(3) . . ?
C11B C12B H12C 111 . . ?
N4 C12B H12C 111 . . ?
C11B C12B H12D 111 . . ?
N4 C12B H12D 111 . . ?
H12C C12B H12D 109 . . ?
O6A C13 O5 117(2) . . ?
O6A C13 O6B 43(2) . . ?
O5 C13 O6B 121(2) . . ?
O6A C13 C14 120(2) . . ?
O5 C13 C14 116(2) . . ?
O6B C13 C14 120(2) . . ?
N5 C14 C13 109.3(18) . . ?
N5 C14 C15 109.1(19) . . ?
C13 C14 C15 115.6(18) . . ?
N5 C14 H14 107.5 . . ?
C13 C14 H14 107.5 . . ?
C15 C14 H14 107.5 . . ?
C16 C15 C14 113.4(18) . . ?
C16 C15 H15A 108.9 . . ?
C14 C15 H15A 108.9 . . ?
C16 C15 H15B 108.9 . . ?
C14 C15 H15B 108.9 . . ?
H15A C15 H15B 107.7 . . ?
C15 C16 C17 111.7(19) . . ?
C15 C16 H16A 109.3 . . ?
C17 C16 H16A 109.3 . . ?
C15 C16 H16B 109.3 . . ?
C17 C16 H16B 109.3 . . ?
H16A C16 H16B 107.9 . . ?
C16 C17 C18 112.6(19) . . ?
C16 C17 H17A 109.1 . . ?
C18 C17 H17A 109.1 . . ?
C16 C17 H17B 109.1 . . ?
C18 C17 H17B 109.1 . . ?
H17A C17 H17B 107.8 . . ?
N6 C18 C17 113.6(17) . . ?
N6 C18 H18A 108.8 . . ?
C17 C18 H18A 108.8 . . ?
N6 C18 H18B 108.8 . . ?
C17 C18 H18B 108.8 . . ?
H18A C18 H18B 107.7 . . ?
C2 N1 H1A 109.5 . . ?
C2 N1 H1B 109.5 . . ?
H1A N1 H1B 109.5 . . ?
C2 N1 H1C 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C6 N2 H2A 109.5 . . ?
C6 N2 H2B 109.5 . . ?
H2A N2 H2B 109.5 . . ?
C6 N2 H2C 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
C8 N3 H3A 109.5 . . ?
C8 N3 H3B 109.5 . . ?
H3A N3 H3B 109.5 . . ?
C8 N3 H3C 109.5 . . ?
H3A N3 H3C 109.5 . . ?
H3B N3 H3C 109.5 . . ?
C12A N4 H4C 109.5 . . ?
C12A N4 H4D 109.5 . . ?
H4C N4 H4D 109.5 . . ?
C12A N4 H4E 109.5 . . ?
H4C N4 H4E 109.5 . . ?
H4D N4 H4E 109.5 . . ?
C12B N4 H4F 109.5 . . ?
C12B N4 H4G 109.5 . . ?
H4F N4 H4G 109.5 . . ?
C12B N4 H4H 109.5 . . ?
H4F N4 H4H 109.5 . . ?
H4G N4 H4H 109.5 . . ?
C14 N5 H5A 109.5 . . ?
C14 N5 H5B 109.5 . . ?
H5A N5 H5B 109.5 . . ?
C14 N5 H5C 109.5 . . ?
H5A N5 H5C 109.5 . . ?
H5B N5 H5C 109.5 . . ?
C18 N6 H6A 109.5 . . ?
C18 N6 H6B 109.5 . . ?
H6A N6 H6B 109.5 . . ?
C18 N6 H6C 109.5 . . ?
H6A N6 H6C 109.5 . . ?
H6B N6 H6C 109.5 . . ?
C1 O1 H1 109.5 . . ?
C7 O3 H3 109.5 . . ?
C13 O5 H5 109.5 . . ?
O6B O6A C13 73(4) . . ?
O6A O6B C13 64(3) . . ?
H7A O7 H7B 109.5 . . ?
PB2 BR2 PB1 159.06(8) . . ?
PB2 BR6 PB1 144.56(9) . 1_565 ?
BR7B BR7A PB2 49.4(8) . . ?
BR7A BR7B PB2 120.0(10) . . ?
PB2 BR8 PB2 153.96(11) 2 . ?
BR1 PB1 BR4 91.69(7) . . ?
BR1 PB1 BR5 92.39(7) . . ?
BR4 PB1 BR5 85.63(6) . . ?
BR1 PB1 BR3 95.99(7) . . ?
BR4 PB1 BR3 87.92(5) . . ?
BR5 PB1 BR3 169.57(7) . . ?
BR1 PB1 BR6 177.13(7) . 1_545 ?
BR4 PB1 BR6 87.53(6) . 1_545 ?
BR5 PB1 BR6 84.80(6) . 1_545 ?
BR3 PB1 BR6 86.75(6) . 1_545 ?
BR1 PB1 BR2 100.72(7) . . ?
BR4 PB1 BR2 165.85(6) . . ?
BR5 PB1 BR2 100.49(6) . . ?
BR3 PB1 BR2 84.07(5) . . ?
BR6 PB1 BR2 80.40(6) 1_545 . ?
BR7B PB2 BR2 91.0(4) . . ?
BR7B PB2 BR6 93.6(2) . . ?
BR2 PB2 BR6 93.54(6) . . ?
BR7B PB2 BR8 92.9(3) . 2_545 ?
BR2 PB2 BR8 91.25(7) . 2_545 ?
BR6 PB2 BR8 171.90(8) . 2_545 ?
BR7B PB2 BR8 89.8(4) . . ?
BR2 PB2 BR8 179.00(7) . . ?
BR6 PB2 BR8 86.95(7) . . ?
BR8 PB2 BR8 88.17(3) 2_545 . ?
BR7B PB2 BR9 177.3(4) . . ?
BR2 PB2 BR9 90.46(6) . . ?
BR6 PB2 BR9 88.67(7) . . ?
BR8 PB2 BR9 84.76(8) 2_545 . ?
BR8 PB2 BR9 88.68(8) . . ?
BR7B PB2 BR7A 10.6(2) . . ?
BR2 PB2 BR7A 81.5(3) . . ?
BR6 PB2 BR7A 89.47(15) . . ?
BR8 PB2 BR7A 97.71(16) 2_545 . ?
BR8 PB2 BR7A 99.4(3) . . ?
BR9 PB2 BR7A 171.6(3) . . ?


# start Validation Reply Form
_vrf_PLAT971_I                   
;
PROBLEM: Check Calcd Resid. Dens.  0.93A   From Pb1             3.68 eA-3  
RESPONSE: This residual density peak is near the heavy atom and can not be
 assigned to unaccounted atom type or twinning error.
;
_vrf_PLAT972_I                   
;
PROBLEM: Check Calcd Resid. Dens.  1.01A   From Pb2            -3.62 eA-3  
RESPONSE: This residual density peak is near the heavy atom and can not be
 assigned to unaccounted atom type or twinning error.
;
_vrf_PLAT973_I                   
;
PROBLEM: Check Calcd Positive Resid. Density on       Pb1       2.03 eA-3  
RESPONSE: This residual density peak is near the heavy atom and can not be
 assigned to unaccounted atom type or twinning error.
;
# end Validation Reply Form

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
