# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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_1-MPPbBr2_1_a
_database_code_depnum_ccdc_archive 'CCDC 1894789'
loop_
_audit_author_name
_audit_author_address
'Mi-Hee Jung'
;Department of Nanotechnology and Advanced Materials Engineering, Sejong University
South Korea
;
_audit_update_record             
;
2019-08-15 deposited with the CCDC.	2019-09-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H28 Br6 N4 Pb'
_chemical_formula_weight         891.01

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0064 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2192 2.4085 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.1439 9.9644 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 2/n'
_space_group_name_Hall           '-P 2yac'

_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+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z-1/2'

_cell_length_a                   9.6500(19)
_cell_length_b                   8.6450(17)
_cell_length_c                   15.562(3)
_cell_angle_alpha                90
_cell_angle_beta                 98.62(3)
_cell_angle_gamma                90
_cell_volume                     1283.6(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    40308
_cell_measurement_theta_min      0.350
_cell_measurement_theta_max      33.679

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.305
_exptl_crystal_F_000             816
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    15.283
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.600
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'HKL3000sm Scalepack(Otwinowski et.al,2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.700
_diffrn_radiation_type           synchrotron
_diffrn_source                   'PLSII 2D bending magnet'
_diffrn_measurement_device_type  'Rayonix MX225HS CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22313
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.302
_diffrn_reflns_theta_max         39.499
_diffrn_reflns_theta_full        24.835
_diffrn_measured_fraction_theta_max 0.763
_diffrn_measured_fraction_theta_full 0.952
_diffrn_reflns_Laue_measured_fraction_max 0.763
_diffrn_reflns_Laue_measured_fraction_full 0.952
_diffrn_reflns_point_group_measured_fraction_max 0.763
_diffrn_reflns_point_group_measured_fraction_full 0.952
_reflns_number_total             6168
_reflns_number_gt                5466
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1982P)²+0.6723P] 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-2017/1 (Sheldrick 2017)'
_refine_ls_extinction_coef       0.0148(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         6168
_refine_ls_number_parameters     98
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0847
_refine_ls_R_factor_gt           0.0812
_refine_ls_wR_factor_ref         0.2582
_refine_ls_wR_factor_gt          0.2503
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_restrained_S_all      1.121
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.250000 0.19380(2) 0.250000 0.03640(13) Uani 1 2 d S T P . .
Br1 Br 0.47142(7) 0.43373(9) 0.28641(5) 0.04960(18) Uani 1 1 d . . . . .
Br2 Br 0.04012(7) -0.07388(8) 0.22762(6) 0.05263(19) Uani 1 1 d . . . . .
Br3 Br 0.26327(9) 0.21666(11) 0.05769(5) 0.0541(2) Uani 1 1 d . . . . .
C1 C 0.2065(19) 0.879(3) 0.6257(12) 0.129(8) Uani 1 1 d . . . . .
H1A H 0.113310 0.867004 0.639305 0.193 Uiso 1 1 calc R U . . .
H1AB H 0.220961 0.985070 0.610711 0.193 Uiso 1 1 calc R U . . .
H1AC H 0.273337 0.850794 0.675187 0.193 Uiso 1 1 calc R U . . .
C2 C 0.3638(7) 0.8077(7) 0.5263(6) 0.0457(13) Uani 1 1 d . . . . .
H2A H 0.434746 0.807793 0.577582 0.055 Uiso 1 1 calc R U . . .
H2AB H 0.364726 0.908018 0.498495 0.055 Uiso 1 1 calc R U . . .
C3 C 0.3953(8) 0.6822(10) 0.4643(7) 0.0570(19) Uani 1 1 d . . . . .
H3A H 0.486376 0.700813 0.447088 0.068 Uiso 1 1 calc R U . . .
H3AB H 0.398373 0.582655 0.493348 0.068 Uiso 1 1 calc R U . . .
C4 C 0.1427(8) 0.6600(9) 0.4079(5) 0.0486(12) Uani 1 1 d . . . . .
H4A H 0.133993 0.557585 0.432028 0.058 Uiso 1 1 calc R U . . .
H4AB H 0.073767 0.669332 0.355992 0.058 Uiso 1 1 calc R U . . .
C5 C 0.1146(7) 0.7792(10) 0.4727(5) 0.0489(13) Uani 1 1 d . . . . .
H5A H 0.023822 0.759341 0.490140 0.059 Uiso 1 1 calc R U . . .
H5AB H 0.111235 0.880601 0.445810 0.059 Uiso 1 1 calc R U . . .
N1 N 0.2848(9) 0.6790(8) 0.3848(5) 0.0544(15) Uani 1 1 d . . . . .
H1B H 0.288405 0.766793 0.355314 0.065 Uiso 1 1 calc R U . . .
H1C H 0.302458 0.601367 0.350504 0.065 Uiso 1 1 calc R U . . .
N2 N 0.2246(6) 0.7787(8) 0.5515(4) 0.0474(11) Uani 1 1 d . . . . .
H2 H 0.227612 0.672625 0.573913 0.057 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br1 2.9707(8) 2 ?
Pb1 Br1 2.9708(8) . ?
Pb1 Br3 3.0211(10) . ?
Pb1 Br3 3.0211(10) 2 ?
Pb1 Br2 3.0605(8) 2 ?
Pb1 Br2 3.0605(8) . ?
C1 N2 1.475(14) . ?
C2 N2 1.476(9) . ?
C2 C3 1.513(11) . ?
C3 N1 1.508(13) . ?
C4 N1 1.478(11) . ?
C4 C5 1.495(11) . ?
C5 N2 1.497(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br1 Pb1 Br1 91.44(4) 2 . ?
Br1 Pb1 Br3 84.34(3) 2 . ?
Br1 Pb1 Br3 90.41(3) . . ?
Br1 Pb1 Br3 90.41(3) 2 2 ?
Br1 Pb1 Br3 84.34(3) . 2 ?
Br3 Pb1 Br3 172.50(4) . 2 ?
Br1 Pb1 Br2 173.92(2) 2 2 ?
Br1 Pb1 Br2 93.52(3) . 2 ?
Br3 Pb1 Br2 92.10(3) . 2 ?
Br3 Pb1 Br2 93.57(3) 2 2 ?
Br1 Pb1 Br2 93.52(3) 2 . ?
Br1 Pb1 Br2 173.92(2) . . ?
Br3 Pb1 Br2 93.57(3) . . ?
Br3 Pb1 Br2 92.10(3) 2 . ?
Br2 Pb1 Br2 81.75(3) 2 . ?
N2 C2 C3 109.0(6) . . ?
N1 C3 C2 110.6(6) . . ?
N1 C4 C5 110.9(6) . . ?
C4 C5 N2 111.9(6) . . ?
C4 N1 C3 111.7(6) . . ?
C1 N2 C2 109.1(8) . . ?
C1 N2 C5 119.1(11) . . ?
C2 N2 C5 110.1(6) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1B Br2 0.89 2.63 3.371(7) 140.7 2_565 yes
N1 H1C Br1 0.89 2.50 3.303(7) 150.7 . yes

_refine_diff_density_max         8.338
_refine_diff_density_min         -4.229
_refine_diff_density_rms         0.479

####################################################################### 
# 
# 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_TDPbBr2_1_a
_database_code_depnum_ccdc_archive 'CCDC 1894790'
loop_
_audit_author_name
_audit_author_address
'Mi-Hee Jung'
;Department of Nanotechnology and Advanced Materials Engineering, Sejong University
South Korea
;
_audit_update_record             
;
2019-08-15 deposited with the CCDC.	2019-09-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C7 H20 Br3 N O2 Pb S2'
_chemical_formula_weight         661.28

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   13.5079(4)
_cell_length_b                   14.8779(4)
_cell_length_c                   9.2938(3)
_cell_angle_alpha                90
_cell_angle_beta                 108.392(2)
_cell_angle_gamma                90
_cell_volume                     1772.36(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    20614
_cell_measurement_theta_min      3.166
_cell_measurement_theta_max      26.8975

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.478
_exptl_crystal_F_000             1216
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    16.507
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.3754
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19782
_diffrn_reflns_av_unetI/netI     0.0478
_diffrn_reflns_av_R_equivalents  0.0492
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.097
_diffrn_reflns_theta_max         28.393
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4414
_reflns_number_gt                3249
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART APEXll'
_computing_cell_refinement       'Bruker SMART APEXll'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1469P)²+40.6124P] 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     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4414
_refine_ls_number_parameters     150
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0437
_refine_ls_wR_factor_ref         0.1552
_refine_ls_wR_factor_gt          0.1255
_refine_ls_goodness_of_fit_ref   0.633
_refine_ls_restrained_S_all      0.633
_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
Pb1 Pb 0.78578(3) 0.76526(2) 0.65484(4) 0.03353(14) Uani 1 1 d . . . . .
Br1 Br 0.94071(9) 0.75806(8) 0.95236(14) 0.0514(3) Uani 1 1 d . . . . .
Br2 Br 0.77733(11) 0.95657(8) 0.67489(14) 0.0656(4) Uani 1 1 d . . . . .
N2 N 0.6045(6) 0.5042(5) 0.5976(9) 0.0380(18) Uani 1 1 d . . . . .
H2A H 0.658168 0.534883 0.658001 0.046 Uiso 1 1 calc R U . . .
H2B H 0.624489 0.447364 0.595606 0.046 Uiso 1 1 calc R U . . .
Br3 Br 0.62109(10) 0.73410(8) 0.78449(17) 0.0573(3) Uani 1 1 d . . . . .
C3 C 0.5758(7) 0.5420(6) 0.4432(10) 0.0362(19) Uani 1 1 d . . . . .
H3A H 0.634928 0.537991 0.405574 0.043 Uiso 1 1 calc R U . . .
H3B H 0.557717 0.604920 0.445880 0.043 Uiso 1 1 calc R U . . .
C4 C 0.5148(8) 0.5079(6) 0.6611(10) 0.039(2) Uani 1 1 d . . . . .
H4 H 0.495049 0.570747 0.668208 0.047 Uiso 1 1 calc R U . . .
C5 C 0.5491(11) 0.4656(9) 0.8197(12) 0.061(3) Uani 1 1 d . . . . .
H5A H 0.488880 0.454354 0.850765 0.091 Uiso 1 1 calc R U . . .
H5B H 0.595254 0.506026 0.890243 0.091 Uiso 1 1 calc R U . . .
H5C H 0.584644 0.410027 0.817396 0.091 Uiso 1 1 calc R U . . .
S1 S 0.90103(19) 0.53839(18) 0.7344(4) 0.0528(7) Uani 1 1 d . . . . .
O1 O 0.7960(5) 0.5860(5) 0.6862(9) 0.0475(18) Uani 1 1 d . . . . .
C1S C 0.8868(12) 0.4547(10) 0.8603(15) 0.073(4) Uani 1 1 d . . . . .
H1S1 H 0.872804 0.482337 0.945157 0.109 Uiso 1 1 calc R U . . .
H1S2 H 0.949997 0.420196 0.895575 0.109 Uiso 1 1 calc R U . . .
H1S3 H 0.829978 0.415761 0.808876 0.109 Uiso 1 1 calc R U . . .
C2S C 0.8991(12) 0.4674(10) 0.5801(16) 0.070(4) Uani 1 1 d . . . . .
H2S1 H 0.843345 0.424731 0.563614 0.105 Uiso 1 1 calc R U . . .
H2S2 H 0.964359 0.436081 0.602772 0.105 Uiso 1 1 calc R U . . .
H2S3 H 0.888580 0.503090 0.490415 0.105 Uiso 1 1 calc R U . . .
S2 S 0.7024(3) 0.23764(19) 0.5646(4) 0.0508(7) Uani 1 1 d . . . . .
O2 O 0.6843(8) 0.3345(7) 0.5817(13) 0.082(3) Uani 1 1 d . . . . .
C3S C 0.8228(10) 0.2118(10) 0.704(2) 0.076(4) Uani 1 1 d . . . . .
H3S1 H 0.877907 0.244831 0.683922 0.115 Uiso 1 1 calc R U . . .
H3S2 H 0.836264 0.148536 0.702119 0.115 Uiso 1 1 calc R U . . .
H3S3 H 0.819272 0.228001 0.802591 0.115 Uiso 1 1 calc R U . . .
C4S C 0.6182(10) 0.1766(9) 0.6397(16) 0.063(3) Uani 1 1 d . . . . .
H4S1 H 0.632401 0.191984 0.744621 0.094 Uiso 1 1 calc R U . . .
H4S2 H 0.629305 0.113422 0.630872 0.094 Uiso 1 1 calc R U . . .
H4S3 H 0.547154 0.191296 0.584580 0.094 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 O1 2.681(7) . ?
Pb1 Br2 2.8569(13) . ?
Pb1 Br3 2.8822(12) . ?
Pb1 Br1 2.8957(12) . ?
N2 C3 1.474(11) . ?
N2 C4 1.506(13) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
C3 C4 1.497(12) 3_666 ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.534(14) . ?
C4 H4 0.9800 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
S1 O1 1.521(7) . ?
S1 C1S 1.761(15) . ?
S1 C2S 1.775(14) . ?
C1S H1S1 0.9600 . ?
C1S H1S2 0.9600 . ?
C1S H1S3 0.9600 . ?
C2S H2S1 0.9600 . ?
C2S H2S2 0.9600 . ?
C2S H2S3 0.9600 . ?
S2 O2 1.479(10) . ?
S2 C4S 1.762(12) . ?
S2 C3S 1.774(15) . ?
C3S H3S1 0.9600 . ?
C3S H3S2 0.9600 . ?
C3S H3S3 0.9600 . ?
C4S H4S1 0.9600 . ?
C4S H4S2 0.9600 . ?
C4S H4S3 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Pb1 Br2 170.22(18) . . ?
O1 Pb1 Br3 79.33(15) . . ?
Br2 Pb1 Br3 94.65(4) . . ?
O1 Pb1 Br1 82.09(16) . . ?
Br2 Pb1 Br1 90.36(4) . . ?
Br3 Pb1 Br1 90.89(4) . . ?
C3 N2 C4 111.7(7) . . ?
C3 N2 H2A 109.3 . . ?
C4 N2 H2A 109.3 . . ?
C3 N2 H2B 109.3 . . ?
C4 N2 H2B 109.3 . . ?
H2A N2 H2B 107.9 . . ?
N2 C3 C4 110.6(7) . 3_666 ?
N2 C3 H3A 109.5 . . ?
C4 C3 H3A 109.5 3_666 . ?
N2 C3 H3B 109.5 . . ?
C4 C3 H3B 109.5 3_666 . ?
H3A C3 H3B 108.1 . . ?
C3 C4 N2 108.8(8) 3_666 . ?
C3 C4 C5 110.8(9) 3_666 . ?
N2 C4 C5 109.0(8) . . ?
C3 C4 H4 109.4 3_666 . ?
N2 C4 H4 109.4 . . ?
C5 C4 H4 109.4 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O1 S1 C1S 103.8(6) . . ?
O1 S1 C2S 105.3(6) . . ?
C1S S1 C2S 98.0(7) . . ?
S1 O1 Pb1 120.5(4) . . ?
S1 C1S H1S1 109.5 . . ?
S1 C1S H1S2 109.5 . . ?
H1S1 C1S H1S2 109.5 . . ?
S1 C1S H1S3 109.5 . . ?
H1S1 C1S H1S3 109.5 . . ?
H1S2 C1S H1S3 109.5 . . ?
S1 C2S H2S1 109.5 . . ?
S1 C2S H2S2 109.5 . . ?
H2S1 C2S H2S2 109.5 . . ?
S1 C2S H2S3 109.5 . . ?
H2S1 C2S H2S3 109.5 . . ?
H2S2 C2S H2S3 109.5 . . ?
O2 S2 C4S 108.0(6) . . ?
O2 S2 C3S 106.1(7) . . ?
C4S S2 C3S 98.9(7) . . ?
S2 C3S H3S1 109.5 . . ?
S2 C3S H3S2 109.5 . . ?
H3S1 C3S H3S2 109.5 . . ?
S2 C3S H3S3 109.5 . . ?
H3S1 C3S H3S3 109.5 . . ?
H3S2 C3S H3S3 109.5 . . ?
S2 C4S H4S1 109.5 . . ?
S2 C4S H4S2 109.5 . . ?
H4S1 C4S H4S2 109.5 . . ?
S2 C4S H4S3 109.5 . . ?
H4S1 C4S H4S3 109.5 . . ?
H4S2 C4S H4S3 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N2 H2A O1 0.89 1.95 2.741(10) 146.9 . yes
N2 H2B O2 0.89 1.89 2.768(13) 170.9 . yes

_refine_diff_density_max         4.039
_refine_diff_density_min         -1.532
_refine_diff_density_rms         0.214

####################################################################### 
# 
# 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_Br_a
_database_code_depnum_ccdc_archive 'CCDC 1894791'
loop_
_audit_author_name
_audit_author_address
'Mi-Hee Jung'
;Department of Nanotechnology and Advanced Materials Engineering, Sejong University
South Korea
;
_audit_update_record             
;
2019-08-15 deposited with the CCDC.	2019-09-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C8 H24 Br6 N4 Pb'
_chemical_formula_weight         862.96

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0021 0.0012 '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 0.0044 0.0024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br 0.0905 1.9124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -1.6071 8.0232 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           58
_space_group_name_H-M_alt        'P n n m'
_space_group_name_Hall           '-P 2 2n'

_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, z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'x-1/2, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   26.499(5)
_cell_length_b                   8.4990(17)
_cell_length_c                   9.805(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2208.2(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    73541
_cell_measurement_theta_min      0.350
_cell_measurement_theta_max      33.679

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.596
_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    12.404
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.711
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'HKL3000sm Scalepack(Otwinowski et.al,2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.610
_diffrn_radiation_type           synchrotron
_diffrn_source                   'PLSII 2D bending magnet'
_diffrn_measurement_device_type  'Rayonix MX225HS CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            37410
_diffrn_reflns_av_unetI/netI     0.0498
_diffrn_reflns_av_R_equivalents  0.1022
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.319
_diffrn_reflns_theta_max         33.641
_diffrn_reflns_theta_full        21.469
_diffrn_measured_fraction_theta_max 0.840
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.840
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.840
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             6078
_reflns_number_gt                3613
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'PAL BL2D-SMDC Program (Shin et. al, 2016)'
_computing_cell_refinement       'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)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-2017/1 (Sheldrick 2017)'
_refine_ls_extinction_coef       0.0011(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         6078
_refine_ls_number_parameters     100
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1039
_refine_ls_R_factor_gt           0.0730
_refine_ls_wR_factor_ref         0.2687
_refine_ls_wR_factor_gt          0.2521
_refine_ls_goodness_of_fit_ref   1.462
_refine_ls_restrained_S_all      1.462
_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
Pb1 Pb 0.62128(2) 0.54631(4) 0.500000 0.04619(15) Uani 1 2 d S T P . .
Br1 Br 0.63266(4) 0.27879(11) 0.29162(10) 0.0616(2) Uani 1 1 d . . . . .
Br2 Br 0.72859(4) 0.60728(14) 0.500000 0.0532(3) Uani 1 2 d S T P . .
Br3 Br 0.61396(3) 0.79656(12) 0.70501(10) 0.0613(2) Uani 1 1 d . . . . .
Br4 Br 0.500000 0.500000 0.500000 0.0527(3) Uani 1 4 d S T P . .
Br5 Br 0.500000 1.000000 0.000000 0.0964(9) Uani 1 4 d S T P . .
C1 C 0.7598(4) 0.5269(10) 0.1241(8) 0.0542(18) Uani 1 1 d . . . . .
H1A H 0.781241 0.518414 0.204024 0.065 Uiso 1 1 calc R U . . .
H1AB H 0.735205 0.442526 0.127415 0.065 Uiso 1 1 calc R U . . .
N6 N 0.5327(4) 0.6370(11) 0.000000 0.053(2) Uani 1 2 d S T P . .
H6A H 0.536060 0.741146 0.000000 0.064 Uiso 1 2 calc R U P . .
H6AB H 0.563389 0.594488 0.000002 0.064 Uiso 1 2 calc R U P . .
C2 C 0.7319(3) 0.6901(11) 0.1250(8) 0.0576(18) Uani 1 1 d . . . . .
H2A H 0.709846 0.696727 0.203675 0.069 Uiso 1 1 calc R U . . .
H2AB H 0.756450 0.774624 0.130965 0.069 Uiso 1 1 calc R U . . .
C3 C 0.5167(3) 1.0665(10) 0.6276(8) 0.0502(16) Uani 1 1 d . . . . .
H3A H 0.538670 1.060763 0.706526 0.060 Uiso 1 1 calc R U . . .
H3AB H 0.497004 1.162385 0.634605 0.060 Uiso 1 1 calc R U . . .
C4 C 0.5046(3) 0.5861(11) 0.1253(9) 0.0586(19) Uani 1 1 d . . . . .
H4A H 0.524015 0.614301 0.205551 0.070 Uiso 1 1 calc R U . . .
H4AB H 0.472602 0.641169 0.129625 0.070 Uiso 1 1 calc R U . . .
N1 N 0.7907(3) 0.5119(11) 0.000000 0.053(2) Uani 1 2 d S T P . .
H1B H 0.805968 0.418653 0.000000 0.063 Uiso 1 2 calc R U P . .
H1C H 0.814374 0.586004 0.000000 0.063 Uiso 1 2 calc R U P . .
N2 N 0.7025(3) 0.7062(12) 0.000000 0.0507(19) Uani 1 2 d S T P . .
H2B H 0.687612 0.800061 -0.000001 0.061 Uiso 1 2 calc R U P . .
H2C H 0.678280 0.633556 0.000000 0.061 Uiso 1 2 calc R U P . .
N5 N 0.5482(3) 1.0720(11) 0.500000 0.056(2) Uani 1 2 d S T P . .
H5B H 0.566438 1.160013 0.500000 0.067 Uiso 1 2 calc R U P . .
H5C H 0.569501 0.991004 0.500002 0.067 Uiso 1 2 calc R U P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br2 2.8906(12) . ?
Pb1 Br3 2.9329(10) . ?
Pb1 Br3 2.9329(10) 6_556 ?
Pb1 Br1 3.0716(11) . ?
Pb1 Br1 3.0716(11) 6_556 ?
Pb1 Br4 3.2377(7) . ?
C1 N1 1.472(10) . ?
C1 C2 1.571(12) . ?
N6 C4 1.499(10) 6 ?
N6 C4 1.499(10) . ?
C2 N2 1.460(9) . ?
C3 C3 1.434(16) 2_675 ?
C3 N5 1.506(9) . ?
C4 C4 1.484(19) 2_665 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br2 Pb1 Br3 86.27(3) . . ?
Br2 Pb1 Br3 86.27(3) . 6_556 ?
Br3 Pb1 Br3 86.53(5) . 6_556 ?
Br2 Pb1 Br1 92.07(3) . . ?
Br3 Pb1 Br1 177.66(3) . . ?
Br3 Pb1 Br1 95.01(3) 6_556 . ?
Br2 Pb1 Br1 92.07(3) . 6_556 ?
Br3 Pb1 Br1 95.01(3) . 6_556 ?
Br3 Pb1 Br1 177.66(3) 6_556 6_556 ?
Br1 Pb1 Br1 83.39(4) . 6_556 ?
Br2 Pb1 Br4 176.66(3) . . ?
Br3 Pb1 Br4 91.292(19) . . ?
Br3 Pb1 Br4 91.292(19) 6_556 . ?
Br1 Pb1 Br4 90.43(2) . . ?
Br1 Pb1 Br4 90.43(2) 6_556 . ?
Pb1 Br4 Pb1 180.0 . 5_666 ?
N1 C1 C2 110.0(7) . . ?
C4 N6 C4 110.0(9) 6 . ?
N2 C2 C1 109.2(7) . . ?
C3 C3 N5 111.5(6) 2_675 . ?
C4 C4 N6 111.5(7) 2_665 . ?
C1 N1 C1 111.6(9) . 6 ?
C2 N2 C2 114.2(8) . 6 ?
C3 N5 C3 112.4(8) 6_556 . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1B Br2 0.89 2.80 3.476(10) 133.8 3_645 yes
N1 H1B Br3 0.89 3.10 3.712(7) 127.6 3_645 yes
N1 H1B Br3 0.89 3.10 3.712(7) 127.6 8_755 yes
N1 H1C Br1 0.89 2.97 3.668(8) 136.4 3_655 yes
N1 H1C Br1 0.89 2.97 3.668(8) 136.4 8_765 yes
N5 H5B Br1 0.89 2.88 3.503(7) 128.7 1_565 yes
N5 H5B Br1 0.89 2.88 3.503(7) 128.7 6_566 yes
N5 H5C Br3 0.89 2.86 3.544(8) 135.1 . yes
N5 H5C Br3 0.89 2.86 3.544(8) 135.1 6_556 yes

_refine_diff_density_max         9.632
_refine_diff_density_min         -3.169
_refine_diff_density_rms         0.397

####################################################################### 
# 
# 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_TDPbBr2_2_a
_database_code_depnum_ccdc_archive 'CCDC 1947298'
loop_
_audit_author_name
_audit_author_address
'Mi-Hee Jung'
;Department of Nanotechnology and Advanced Materials Engineering, Sejong University
South Korea
;
_audit_update_record             
;
2019-08-15 deposited with the CCDC.	2019-09-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C8 H22 Br3 N2 O Pb S'
_chemical_formula_weight         641.25

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'
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'
S S 0.3331 0.5567 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

_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+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   18.9362(4)
_cell_length_b                   8.7005(2)
_cell_length_c                   19.8672(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3273.21(12)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9276
_cell_measurement_theta_min      4.6390
_cell_measurement_theta_max      73.7790

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.603
_exptl_crystal_F_000             2360
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    29.709
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16772
_diffrn_reflns_av_unetI/netI     0.0460
_diffrn_reflns_av_R_equivalents  0.0785
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         4.451
_diffrn_reflns_theta_max         74.405
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3247
_reflns_number_gt                3007
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1319P)²+36.6300P] 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     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3247
_refine_ls_number_parameters     149
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0610
_refine_ls_wR_factor_ref         0.1826
_refine_ls_wR_factor_gt          0.1797
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.053
_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
Pb1 Pb 0.49841(2) 0.33935(5) 0.24346(2) 0.0104(2) Uani 1 1 d . . . . .
N1 N 0.5966(4) 0.4072(9) 0.3480(4) 0.0123(15) Uani 1 1 d . . . . .
H1A* H 0.587895 0.505959 0.339731 0.015 Uiso 1 1 calc R U . . .
H1B H 0.572566 0.351172 0.318318 0.015 Uiso 1 1 calc R U . . .
C1 C 0.5666(5) 0.1648(12) 0.5058(5) 0.023(2) Uani 1 1 d . . . . .
H1A H 0.516478 0.175869 0.511485 0.034 Uiso 1 1 calc R U . . .
H1AB H 0.590629 0.234465 0.535420 0.034 Uiso 1 1 calc R U . . .
H1AC H 0.580143 0.061199 0.516214 0.034 Uiso 1 1 calc R U . . .
Br1 Br 0.43531(6) 0.10788(14) 0.33076(6) 0.0268(3) Uani 1 1 d . . . . .
Br2 Br 0.41810(5) 0.56763(11) 0.32005(5) 0.0174(3) Uani 1 1 d . . . . .
N2 N 0.6626(4) 0.1627(8) 0.4206(4) 0.0136(16) Uani 1 1 d . . . . .
H2A H 0.689234 0.210775 0.450990 0.016 Uiso 1 1 calc R U . . .
H2B H 0.668909 0.062043 0.426008 0.016 Uiso 1 1 calc R U . . .
C2 C 0.5863(4) 0.2011(10) 0.4332(4) 0.0114(16) Uani 1 1 d . . . . .
H2 H 0.557023 0.138028 0.403350 0.014 Uiso 1 1 calc R U . . .
Br3 Br 0.38539(5) 0.31315(11) 0.14271(5) 0.0171(3) Uani 1 1 d . . . . .
C3 C 0.5738(5) 0.3684(11) 0.4166(5) 0.0140(17) Uani 1 1 d . . . . .
H3A H 0.523914 0.391197 0.421270 0.017 Uiso 1 1 calc R U . . .
H3AB H 0.599371 0.431945 0.448475 0.017 Uiso 1 1 calc R U . . .
C7 C 0.6865(5) 0.2074(11) 0.3519(4) 0.0142(17) Uani 1 1 d . . . . .
H7A H 0.661230 0.147523 0.318523 0.017 Uiso 1 1 calc R U . . .
H7AB H 0.736530 0.186292 0.347101 0.017 Uiso 1 1 calc R U . . .
C6 C 0.7001(5) 0.4240(12) 0.2710(5) 0.0172(19) Uani 1 1 d . . . . .
H6A H 0.749415 0.399688 0.267604 0.026 Uiso 1 1 calc R U . . .
H6AB H 0.693567 0.532565 0.265008 0.026 Uiso 1 1 calc R U . . .
H6AC H 0.674416 0.369413 0.236934 0.026 Uiso 1 1 calc R U . . .
C4 C 0.6728(5) 0.3768(10) 0.3406(4) 0.0126(17) Uani 1 1 d . . . . .
H4 H 0.698366 0.435594 0.374912 0.015 Uiso 1 1 calc R U . . .
S1 S 0.69996(11) -0.1599(2) 0.55329(11) 0.0130(5) Uani 1 1 d . . . . .
O1 O 0.7548(3) -0.1460(8) 0.4974(4) 0.0197(15) Uani 1 1 d . . . . .
C1S C 0.6465(5) -0.3219(11) 0.5319(5) 0.0158(18) Uani 1 1 d . . . . .
H1S1 H 0.617859 -0.297259 0.493430 0.024 Uiso 1 1 calc R U . . .
H1S2 H 0.616514 -0.347451 0.569203 0.024 Uiso 1 1 calc R U . . .
H1S3 H 0.676237 -0.407906 0.521400 0.024 Uiso 1 1 calc R U . . .
C2S C 0.7447(5) -0.2449(13) 0.6235(5) 0.021(2) Uani 1 1 d . . . . .
H2S1 H 0.760502 -0.346107 0.611486 0.032 Uiso 1 1 calc R U . . .
H2S2 H 0.712875 -0.251594 0.661009 0.032 Uiso 1 1 calc R U . . .
H2S3 H 0.784555 -0.182689 0.635552 0.032 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br1 2.9140(12) . ?
Pb1 Br2 2.9279(10) . ?
Pb1 Br3 2.9391(10) . ?
Pb1 Br1 3.0345(12) 3_655 ?
Pb1 Br2 3.1115(10) 3_645 ?
N1 C3 1.470(11) . ?
N1 C4 1.474(11) . ?
N1 H1A* 0.8900 . ?
N1 H1B 0.8900 . ?
C1 C2 1.522(12) . ?
C1 H1A 0.9600 . ?
C1 H1AB 0.9600 . ?
C1 H1AC 0.9600 . ?
N2 C7 1.490(11) . ?
N2 C2 1.505(11) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
C2 C3 1.511(12) . ?
C2 H2 0.9800 . ?
C3 H3A 0.9700 . ?
C3 H3AB 0.9700 . ?
C7 C4 1.513(12) . ?
C7 H7A 0.9700 . ?
C7 H7AB 0.9700 . ?
C6 C4 1.532(12) . ?
C6 H6A 0.9600 . ?
C6 H6AB 0.9600 . ?
C6 H6AC 0.9600 . ?
C4 H4 0.9800 . ?
S1 O1 1.524(7) . ?
S1 C1S 1.787(9) . ?
S1 C2S 1.791(10) . ?
C1S H1S1 0.9600 . ?
C1S H1S2 0.9600 . ?
C1S H1S3 0.9600 . ?
C2S H2S1 0.9600 . ?
C2S H2S2 0.9600 . ?
C2S H2S3 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br1 Pb1 Br2 86.94(3) . . ?
Br1 Pb1 Br3 93.05(3) . . ?
Br2 Pb1 Br3 91.63(3) . . ?
Br1 Pb1 Br1 172.27(3) . 3_655 ?
Br2 Pb1 Br1 86.85(3) . 3_655 ?
Br3 Pb1 Br1 91.72(3) . 3_655 ?
Br1 Pb1 Br2 85.67(3) . 3_645 ?
Br2 Pb1 Br2 171.93(3) . 3_645 ?
Br3 Pb1 Br2 92.00(3) . 3_645 ?
Br1 Pb1 Br2 100.24(3) 3_655 3_645 ?
C3 N1 C4 109.8(7) . . ?
C3 N1 H1A* 109.7 . . ?
C4 N1 H1A* 109.7 . . ?
C3 N1 H1B 109.7 . . ?
C4 N1 H1B 109.7 . . ?
H1A* N1 H1B 108.2 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1AB 109.5 . . ?
H1A C1 H1AB 109.5 . . ?
C2 C1 H1AC 109.5 . . ?
H1A C1 H1AC 109.5 . . ?
H1AB C1 H1AC 109.5 . . ?
Pb1 Br1 Pb1 94.20(3) . 3_645 ?
Pb1 Br2 Pb1 92.33(2) . 3_655 ?
C7 N2 C2 112.7(7) . . ?
C7 N2 H2A 109.1 . . ?
C2 N2 H2A 109.1 . . ?
C7 N2 H2B 109.1 . . ?
C2 N2 H2B 109.1 . . ?
H2A N2 H2B 107.8 . . ?
N2 C2 C3 109.1(7) . . ?
N2 C2 C1 110.3(7) . . ?
C3 C2 C1 111.6(8) . . ?
N2 C2 H2 108.6 . . ?
C3 C2 H2 108.6 . . ?
C1 C2 H2 108.6 . . ?
N1 C3 C2 112.2(7) . . ?
N1 C3 H3A 109.2 . . ?
C2 C3 H3A 109.2 . . ?
N1 C3 H3AB 109.2 . . ?
C2 C3 H3AB 109.2 . . ?
H3A C3 H3AB 107.9 . . ?
N2 C7 C4 109.8(7) . . ?
N2 C7 H7A 109.7 . . ?
C4 C7 H7A 109.7 . . ?
N2 C7 H7AB 109.7 . . ?
C4 C7 H7AB 109.7 . . ?
H7A C7 H7AB 108.2 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6AB 109.5 . . ?
H6A C6 H6AB 109.5 . . ?
C4 C6 H6AC 109.5 . . ?
H6A C6 H6AC 109.5 . . ?
H6AB C6 H6AC 109.5 . . ?
N1 C4 C7 109.1(7) . . ?
N1 C4 C6 111.8(7) . . ?
C7 C4 C6 109.7(8) . . ?
N1 C4 H4 108.7 . . ?
C7 C4 H4 108.7 . . ?
C6 C4 H4 108.7 . . ?
O1 S1 C1S 105.9(4) . . ?
O1 S1 C2S 106.1(4) . . ?
C1S S1 C2S 97.3(5) . . ?
S1 C1S H1S1 109.5 . . ?
S1 C1S H1S2 109.5 . . ?
H1S1 C1S H1S2 109.5 . . ?
S1 C1S H1S3 109.5 . . ?
H1S1 C1S H1S3 109.5 . . ?
H1S2 C1S H1S3 109.5 . . ?
S1 C2S H2S1 109.5 . . ?
S1 C2S H2S2 109.5 . . ?
H2S1 C2S H2S2 109.5 . . ?
S1 C2S H2S3 109.5 . . ?
H2S1 C2S H2S3 109.5 . . ?
H2S2 C2S H2S3 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1A* Br3 0.89 2.74 3.553(8) 152.0 3_655 yes
N2 H2A O1 0.89 1.88 2.746(10) 164.6 8_765 yes
N2 H2B Br3 0.89 2.76 3.415(7) 131.6 3_645 yes

_refine_diff_density_max         5.369
_refine_diff_density_min         -3.801
_refine_diff_density_rms         0.538

####################################################################### 
# 
# 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_PPbCl2_2_a
_database_code_depnum_ccdc_archive 'CCDC 1894792'
loop_
_audit_author_name
_audit_author_address
'Mi-Hee Jung'
;Department of Nanotechnology and Advanced Materials Engineering, Sejong University
South Korea
;
_audit_update_record             
;
2019-08-15 deposited with the CCDC.	2019-09-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C8 H24 Cl12 N4 Pb4'
_chemical_formula_weight         1430.47

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0064 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1472 0.1563 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.1439 9.9644 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_H-M_alt        'R 3 :H'
_space_group_name_Hall           'R 3'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'

_cell_length_a                   15.327(2)
_cell_length_b                   15.327(2)
_cell_length_c                   33.107(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     6736(2)
_cell_formula_units_Z            9
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    79868
_cell_measurement_theta_min      0.350
_cell_measurement_theta_max      33.679

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.174
_exptl_crystal_F_000             5688
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    22.450
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.700
_diffrn_radiation_type           synchrotron
_diffrn_source                   'PLSII 2D bending magnet'
_diffrn_measurement_device_type  'Rayonix MX225HS CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            41572
_diffrn_reflns_av_unetI/netI     0.0601
_diffrn_reflns_av_R_equivalents  0.0737
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_theta_min         1.628
_diffrn_reflns_theta_max         39.482
_diffrn_reflns_theta_full        24.835
_diffrn_measured_fraction_theta_max 0.892
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.892
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.892
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             16722
_reflns_number_gt                13169
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_max     0.892
_reflns_Friedel_fraction_full    1.000

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1398P)²+55.9169P] 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-2017/1 (Sheldrick 2017)'
_refine_ls_extinction_coef       0.00143(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.502(19)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         16722
_refine_ls_number_parameters     255
_refine_ls_number_restraints     51
_refine_ls_R_factor_all          0.0851
_refine_ls_R_factor_gt           0.0760
_refine_ls_wR_factor_ref         0.2564
_refine_ls_wR_factor_gt          0.2414
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_restrained_S_all      1.086
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.19950(6) 0.47797(6) 0.60102(2) 0.04662(17) Uani 1 1 d . . . . .
Cl1 Cl 0.333333 0.666667 0.5534(2) 0.0378(11) Uani 1 3 d S T P . .
C1 C 0.5286(11) 0.5734(13) 0.4646(5) 0.058(4) Uani 1 1 d D . . . .
H1A H 0.510516 0.537353 0.439129 0.069 Uiso 1 1 calc R U . . .
H1B H 0.551371 0.643684 0.459097 0.069 Uiso 1 1 calc R U . . .
N1 N 0.4382(16) 0.5313(14) 0.4915(6) 0.24(3) Uani 1 1 d D U . . .
H1C H 0.453099 0.566297 0.514357 0.284 Uiso 1 1 calc R U . . .
H1D H 0.388406 0.535116 0.479302 0.284 Uiso 1 1 calc R U . . .
Pb2 Pb 0.05451(6) 0.18863(6) 0.54221(2) 0.04809(18) Uani 1 1 d . . . . .
C2 C 0.6104(12) 0.5646(13) 0.4835(6) 0.081(9) Uani 1 1 d D . . . .
H2A H 0.635650 0.610563 0.506287 0.097 Uiso 1 1 calc R U . . .
H2B H 0.664867 0.586459 0.464194 0.097 Uiso 1 1 calc R U . . .
Cl2 Cl -0.0297(7) 0.3368(10) 0.5711(4) 0.118(3) Uani 1 1 d . . . . .
N2 N 0.5839(13) 0.4629(11) 0.4980(4) 0.136(16) Uani 1 1 d D . . . .
H2C H 0.576520 0.423154 0.477161 0.163 Uiso 1 1 calc R U . . .
H2D H 0.632496 0.466593 0.513869 0.163 Uiso 1 1 calc R U . . .
C3 C 0.4888(12) 0.422(2) 0.5208(6) 0.093(11) Uani 1 1 d D U . . .
H3A H 0.466195 0.351887 0.527256 0.111 Uiso 1 1 calc R U . . .
H3B H 0.502018 0.458160 0.546047 0.111 Uiso 1 1 calc R U . . .
Pb3 Pb 0.94504(6) 0.81109(6) 0.43437(2) 0.04625(17) Uani 1 1 d . . . . .
Cl3 Cl 0.1895(4) 0.3993(4) 0.52297(14) 0.0469(9) Uani 1 1 d . . . . .
N3 N 0.241(2) 0.203(2) 0.6389(10) 0.28(4) Uani 1 1 d D U . . .
H3C H 0.209083 0.199270 0.615839 0.334 Uiso 1 1 calc R U . . .
H3D H 0.251443 0.258713 0.651598 0.334 Uiso 1 1 calc R U . . .
Pb4 Pb 0.80092(6) 0.52211(6) 0.37554(2) 0.04754(18) Uani 1 1 d . . . . .
Cl4 Cl 0.3807(4) 0.4816(4) 0.61176(19) 0.0548(11) Uani 1 1 d . . . . .
C4 C 0.4072(15) 0.4263(15) 0.5000(9) 0.104(13) Uani 1 1 d D . . . .
H4A H 0.347369 0.396576 0.516800 0.125 Uiso 1 1 calc R U . . .
H4B H 0.391355 0.388531 0.474963 0.125 Uiso 1 1 calc R U . . .
N4 N 0.3392(16) 0.0911(11) 0.6711(7) 0.23(3) Uani 1 1 d D . . . .
H4C H 0.328166 0.041544 0.654215 0.279 Uiso 1 1 calc R U . . .
H4D H 0.368373 0.084425 0.693256 0.279 Uiso 1 1 calc R U . . .
Cl5 Cl 0.000000 0.000000 0.5918(3) 0.0433(13) Uani 1 3 d S T P . .
C5 C 0.338(2) 0.212(2) 0.6294(9) 0.24(5) Uani 1 1 d D . . . .
H5A H 0.380057 0.282548 0.622030 0.294 Uiso 1 1 calc R U . . .
H5B H 0.325854 0.174910 0.604390 0.294 Uiso 1 1 calc R U . . .
Cl6 Cl 0.2309(4) 0.1883(4) 0.53367(18) 0.0515(10) Uani 1 1 d . . . . .
C6 C 0.4064(19) 0.1888(13) 0.6520(9) 0.18(2) Uani 1 1 d D U . . .
H6A H 0.453691 0.183995 0.634009 0.218 Uiso 1 1 calc R U . . .
H6B H 0.443662 0.240039 0.672200 0.218 Uiso 1 1 calc R U . . .
Cl7 Cl 1.000000 1.000000 0.4854(2) 0.0381(8) Uani 1 3 d S T P . .
C7 C 0.2431(19) 0.084(2) 0.6819(8) 0.22(3) Uani 1 1 d D U . . .
H7A H 0.256322 0.114256 0.708612 0.266 Uiso 1 1 calc R U . . .
H7B H 0.199199 0.012532 0.686457 0.266 Uiso 1 1 calc R U . . .
Cl8 Cl 1.000000 1.000000 0.3871(2) 0.0510(18) Uani 1 3 d S T P . .
C8 C 0.1739(6) 0.1153(7) 0.6641(3) 0.0255(13) Uani 1 1 d D . . . .
H8A H 0.122303 0.061668 0.647793 0.031 Uiso 1 1 calc R U . . .
H8B H 0.141727 0.133806 0.684944 0.031 Uiso 1 1 calc R U . . .
Cl09 Cl 0.1206(4) 0.2664(4) 0.61977(13) 0.0451(8) Uani 1 1 d . . . . .
Cl9 Cl 0.7673(4) 0.8140(4) 0.44800(18) 0.0518(10) Uani 1 1 d . . . . .
Cl10 Cl 0.8752(5) 0.7396(4) 0.35660(17) 0.0598(14) Uani 1 1 d . . . . .
Cl11 Cl 1.0338(4) 0.6687(6) 0.4043(2) 0.0647(12) Uani 1 1 d . . . . .
Cl12 Cl 0.8048(5) 0.5931(4) 0.45318(16) 0.0566(13) Uani 1 1 d . . . . .
Cl13 Cl 0.6248(4) 0.5215(4) 0.36419(19) 0.0529(11) Uani 1 1 d . . . . .
Cl14 Cl 0.666667 0.333333 0.4251(3) 0.061(2) Uani 1 3 d S T P . .
Cl15 Cl 0.666667 0.333333 0.3223(3) 0.0401(7) Uani 1 3 d S T P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Cl4 2.774(5) . ?
Pb1 Cl3 2.823(5) . ?
Pb1 Cl09 2.905(5) . ?
Pb1 Cl1 3.021(4) . ?
C1 C2 1.467(13) . ?
C1 N1 1.493(13) . ?
N1 C4 1.460(13) . ?
Pb2 Cl6 2.721(5) . ?
Pb2 Cl09 2.799(5) . ?
Pb2 Cl3 2.904(5) . ?
Pb2 Cl5 3.055(5) . ?
C2 N2 1.480(13) . ?
N2 C3 1.473(13) . ?
C3 C4 1.458(13) . ?
Pb3 Cl9 2.783(5) . ?
Pb3 Cl10 2.793(5) . ?
Pb3 Cl12 2.998(5) . ?
Pb3 Cl8 3.017(4) . ?
Pb3 Cl7 3.084(4) . ?
N3 C5 1.461(14) . ?
N3 C8 1.475(13) . ?
Pb4 Cl13 2.721(6) . ?
Pb4 Cl12 2.780(5) . ?
Pb4 Cl10 3.001(5) . ?
Pb4 Cl14 3.057(5) . ?
N4 C7 1.467(14) . ?
N4 C6 1.470(13) . ?
C5 C6 1.471(14) . ?
C7 C8 1.486(13) . ?

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
Cl4 Pb1 Cl3 88.05(17) . . ?
Cl4 Pb1 Cl09 81.29(17) . . ?
Cl3 Pb1 Cl09 79.38(12) . . ?
Cl4 Pb1 Cl1 81.61(14) . . ?
Cl3 Pb1 Cl1 78.27(14) . . ?
Cl09 Pb1 Cl1 152.18(12) . . ?
Pb1 Cl1 Pb1 95.22(15) . 3_565 ?
Pb1 Cl1 Pb1 95.22(15) . 2_665 ?
Pb1 Cl1 Pb1 95.22(15) 3_565 2_665 ?
C2 C1 N1 110.9(14) . . ?
C4 N1 C1 108.1(15) . . ?
Cl6 Pb2 Cl09 87.01(17) . . ?
Cl6 Pb2 Cl3 79.81(16) . . ?
Cl09 Pb2 Cl3 79.79(13) . . ?
Cl6 Pb2 Cl5 81.73(12) . . ?
Cl09 Pb2 Cl5 77.27(16) . . ?
Cl3 Pb2 Cl5 151.14(14) . . ?
C1 C2 N2 116.0(15) . . ?
C3 N2 C2 108.0(16) . . ?
C4 C3 N2 115.2(15) . . ?
Cl9 Pb3 Cl10 88.3(2) . . ?
Cl9 Pb3 Cl12 79.74(19) . . ?
Cl10 Pb3 Cl12 80.43(14) . . ?
Cl9 Pb3 Cl8 82.81(13) . . ?
Cl10 Pb3 Cl8 76.51(16) . . ?
Cl12 Pb3 Cl8 151.37(15) . . ?
Cl9 Pb3 Cl7 72.92(11) . . ?
Cl10 Pb3 Cl7 138.13(16) . . ?
Cl12 Pb3 Cl7 129.75(14) . . ?
Cl8 Pb3 Cl7 64.48(16) . . ?
Pb1 Cl3 Pb2 97.50(14) . . ?
C5 N3 C8 114.8(19) . . ?
Cl13 Pb4 Cl12 87.5(2) . . ?
Cl13 Pb4 Cl10 78.45(18) . . ?
Cl12 Pb4 Cl10 80.57(14) . . ?
Cl13 Pb4 Cl14 82.74(13) . . ?
Cl12 Pb4 Cl14 75.35(19) . . ?
Cl10 Pb4 Cl14 149.94(17) . . ?
C3 C4 N1 109(2) . . ?
C7 N4 C6 110.2(16) . . ?
Pb2 Cl5 Pb2 93.85(18) 2 3 ?
Pb2 Cl5 Pb2 93.85(18) 2 . ?
Pb2 Cl5 Pb2 93.85(18) 3 . ?
N3 C5 C6 133(3) . . ?
N4 C6 C5 104.3(16) . . ?
Pb3 Cl7 Pb3 92.84(15) . 3_675 ?
Pb3 Cl7 Pb3 92.84(15) . 2_765 ?
Pb3 Cl7 Pb3 92.84(15) 3_675 2_765 ?
N4 C7 C8 137.0(18) . . ?
Pb3 Cl8 Pb3 95.53(16) . 2_765 ?
Pb3 Cl8 Pb3 95.53(16) . 3_675 ?
Pb3 Cl8 Pb3 95.54(16) 2_765 3_675 ?
N3 C8 C7 103.7(14) . . ?
Pb2 Cl09 Pb1 98.01(13) . . ?
Pb3 Cl10 Pb4 95.82(17) . . ?
Pb4 Cl12 Pb3 96.16(17) . . ?
Pb4 Cl14 Pb4 93.9(2) . 3_665 ?
Pb4 Cl14 Pb4 93.9(2) . 2_655 ?
Pb4 Cl14 Pb4 93.9(2) 3_665 2_655 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N2 H2C Cl14 0.89 2.95 3.729(19) 147.7 . yes
N3 H3C Cl6 0.89 2.76 3.49(4) 140.5 . yes
N3 H3C Cl09 0.89 2.08 2.55(3) 112.5 . yes
N4 H4C Cl2 0.89 2.84 3.52(3) 135.1 3 yes
N4 H4C Cl09 0.89 2.89 3.548(18) 132.3 3 yes
N4 H4C Cl13 0.89 2.99 3.430(15) 112.3 4_445 yes
N4 H4D Cl10 0.89 2.75 3.31(2) 122.1 4_445 yes

_refine_diff_density_max         6.973
_refine_diff_density_min         -2.449
_refine_diff_density_rms         0.510

