# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_www
_database_code_depnum_ccdc_archive 'CCDC 1962913'
loop_
_audit_author_name
_audit_author_address
'chai siqian'
;Tianjin university
China
;
_audit_update_record             
;
2020-01-10 deposited with the CCDC.	2020-01-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H24 Cl4 N2 Pb'
_chemical_formula_weight         521.30

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'
Cl Cl 0.3639 0.7018 '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           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

_cell_length_a                   25.0243(15)
_cell_length_b                   6.0344(3)
_cell_length_c                   11.7615(6)
_cell_angle_alpha                90
_cell_angle_beta                 104.112(5)
_cell_angle_gamma                90
_cell_volume                     1722.46(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    373(2)
_cell_measurement_reflns_used    7294
_cell_measurement_theta_min      3.6450
_cell_measurement_theta_max      72.2130

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.010
_exptl_crystal_F_000             992
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.210
_exptl_absorpt_coefficient_mu    24.621
_shelx_estimated_absorpt_T_min   0.055
_shelx_estimated_absorpt_T_max   0.079
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.07150
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      373(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            7651
_diffrn_reflns_av_unetI/netI     0.0935
_diffrn_reflns_av_R_equivalents  0.1733
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.642
_diffrn_reflns_theta_max         73.030
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1690
_reflns_number_gt                1637
_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       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.2200P)²+0.4599P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.0016(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1690
_refine_ls_number_parameters     137
_refine_ls_number_restraints     276
_refine_ls_R_factor_all          0.0959
_refine_ls_R_factor_gt           0.0954
_refine_ls_wR_factor_ref         0.2413
_refine_ls_wR_factor_gt          0.2400
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      0.952
_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 0.500000 0.55274(8) 0.250000 0.0575(5) Uani 1 2 d S T P . .
Cl1 Cl 0.500000 1.0051(16) 0.250000 0.105(2) Uani 1 2 d S T P . .
Cl2 Cl 0.500000 0.500000 0.000000 0.108(2) Uani 1 2 d S . P . .
Cl3 Cl 0.6170(3) 0.5961(13) 0.3092(7) 0.1090(16) Uani 1 1 d . . . . .
N1 N 0.623(3) 1.078(12) 0.473(7) 0.114(15) Uani 0.45(5) 1 d . U P A 1
H1A H 0.607936 1.212651 0.470331 0.137 Uiso 0.45(5) 1 d R U P A 1
H1B H 0.615986 1.027333 0.399684 0.137 Uiso 0.45(5) 1 d R U P A 1
C1 C 0.6843(18) 1.182(8) 0.553(5) 0.087(10) Uani 0.45(5) 1 d . U P A 1
H1C H 0.704497 1.264433 0.505592 0.104 Uiso 0.45(5) 1 calc R U P A 1
H1D H 0.681099 1.267965 0.620373 0.104 Uiso 0.45(5) 1 calc R U P A 1
C2 C 0.709(3) 0.919(11) 0.586(6) 0.093(12) Uani 0.45(5) 1 d . U P A 1
H2A H 0.697878 0.819384 0.519995 0.111 Uiso 0.45(5) 1 calc R U P A 1
H2B H 0.748430 0.916281 0.615820 0.111 Uiso 0.45(5) 1 calc R U P A 1
C3 C 0.680(3) 0.870(15) 0.679(7) 0.121(15) Uani 0.45(5) 1 d . U P A 1
H3A H 0.672764 1.000659 0.720850 0.145 Uiso 0.45(5) 1 calc R U P A 1
H3B H 0.697676 0.755963 0.732827 0.145 Uiso 0.45(5) 1 calc R U P A 1
C4 C 0.626(3) 0.783(11) 0.583(7) 0.111(13) Uani 0.45(5) 1 d . U P A 1
H4A H 0.607061 0.713110 0.636710 0.133 Uiso 0.45(5) 1 d R U P A 1
H4B H 0.623323 0.681758 0.517897 0.133 Uiso 0.45(5) 1 d R U P A 1
C5 C 0.596(2) 1.033(9) 0.568(6) 0.084(12) Uani 0.45(5) 1 d . U P A 1
H5A H 0.560598 0.989845 0.518859 0.101 Uiso 0.45(5) 1 d R U P A 1
H5B H 0.589347 1.116255 0.633638 0.101 Uiso 0.45(5) 1 d R U P A 1
N1' N 0.6209(17) 1.165(7) 0.510(5) 0.103(10) Uani 0.55(5) 1 d . U P A 2
H1'1 H 0.633980 1.177812 0.587555 0.124 Uiso 0.55(5) 1 d R U P A 2
H1'2 H 0.604183 1.287523 0.476996 0.124 Uiso 0.55(5) 1 d R U P A 2
C1' C 0.682(2) 1.094(12) 0.505(6) 0.113(13) Uani 0.55(5) 1 d . U P A 2
H1'3 H 0.678723 0.978113 0.446844 0.135 Uiso 0.55(5) 1 calc R U P A 2
H1'4 H 0.699359 1.220107 0.478882 0.135 Uiso 0.55(5) 1 calc R U P A 2
C2' C 0.712(2) 1.026(10) 0.599(7) 0.103(13) Uani 0.55(5) 1 d . U P A 2
H2'1 H 0.714502 1.137432 0.659864 0.123 Uiso 0.55(5) 1 calc R U P A 2
H2'2 H 0.748375 0.995234 0.589617 0.123 Uiso 0.55(5) 1 calc R U P A 2
C3' C 0.684(2) 0.799(9) 0.635(6) 0.113(12) Uani 0.55(5) 1 d . U P A 2
H3'1 H 0.684112 0.683101 0.578484 0.136 Uiso 0.55(5) 1 calc R U P A 2
H3'2 H 0.704107 0.747590 0.711788 0.136 Uiso 0.55(5) 1 calc R U P A 2
C4' C 0.6229(18) 0.854(8) 0.638(5) 0.098(10) Uani 0.55(5) 1 d . U P A 2
H4'1 H 0.603921 0.733434 0.666215 0.118 Uiso 0.55(5) 1 d R U P A 2
H4'2 H 0.628290 0.979287 0.691705 0.118 Uiso 0.55(5) 1 d R U P A 2
C5' C 0.598(3) 0.949(8) 0.525(7) 0.097(13) Uani 0.55(5) 1 d . U P A 2
H5'1 H 0.558402 0.953287 0.499988 0.117 Uiso 0.55(5) 1 d R U P A 2
H5'2 H 0.614489 0.869855 0.469784 0.117 Uiso 0.55(5) 1 d R U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Cl1 2.730(10) . ?
Pb1 Cl3 2.851(7) . ?
Pb1 Cl3 2.851(7) 2_655 ?
Pb1 Cl2 2.95754(16) . ?
Pb1 Cl2 2.95754(16) 2_655 ?
N1 C5 1.46(10) . ?
N1 C1 1.72(9) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
C1 C2 1.71(9) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C2 C3 1.47(11) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.62(10) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.67(8) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
N1' C5' 1.45(7) . ?
N1' C1' 1.59(8) . ?
N1' H1'1 0.8900 . ?
N1' H1'2 0.8900 . ?
C1' C2' 1.25(9) . ?
C1' H1'3 0.9700 . ?
C1' H1'4 0.9700 . ?
C2' C3' 1.64(7) . ?
C2' H2'1 0.9700 . ?
C2' H2'2 0.9700 . ?
C3' C4' 1.56(7) . ?
C3' H3'1 0.9700 . ?
C3' H3'2 0.9700 . ?
C4' C5' 1.44(8) . ?
C4' H4'1 0.9700 . ?
C4' H4'2 0.9700 . ?
C5' H5'1 0.9700 . ?
C5' H5'2 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1 Pb1 Cl3 84.73(15) . . ?
Cl1 Pb1 Cl3 84.73(15) . 2_655 ?
Cl3 Pb1 Cl3 169.5(3) . 2_655 ?
Cl1 Pb1 Cl2 96.178(9) . . ?
Cl3 Pb1 Cl2 90.22(17) . . ?
Cl3 Pb1 Cl2 90.91(17) 2_655 . ?
Cl1 Pb1 Cl2 96.178(9) . 2_655 ?
Cl3 Pb1 Cl2 90.91(17) . 2_655 ?
Cl3 Pb1 Cl2 90.22(17) 2_655 2_655 ?
Cl2 Pb1 Cl2 167.644(18) . 2_655 ?
Pb1 Cl2 Pb1 180.0 . 5_665 ?
C5 N1 C1 100(6) . . ?
C5 N1 H1A 86.3 . . ?
C1 N1 H1A 89.5 . . ?
C5 N1 H1B 131.7 . . ?
C1 N1 H1B 125.8 . . ?
H1A N1 H1B 107.6 . . ?
C2 C1 N1 90(4) . . ?
C2 C1 H1C 113.6 . . ?
N1 C1 H1C 113.6 . . ?
C2 C1 H1D 113.6 . . ?
N1 C1 H1D 113.6 . . ?
H1C C1 H1D 110.8 . . ?
C3 C2 C1 98(5) . . ?
C3 C2 H2A 112.1 . . ?
C1 C2 H2A 112.1 . . ?
C3 C2 H2B 112.1 . . ?
C1 C2 H2B 112.1 . . ?
H2A C2 H2B 109.7 . . ?
C2 C3 C4 92(6) . . ?
C2 C3 H3A 113.3 . . ?
C4 C3 H3A 113.3 . . ?
C2 C3 H3B 113.3 . . ?
C4 C3 H3B 113.3 . . ?
H3A C3 H3B 110.7 . . ?
C3 C4 C5 93(6) . . ?
C3 C4 H4A 98.5 . . ?
C5 C4 H4A 100.4 . . ?
C3 C4 H4B 129.9 . . ?
C5 C4 H4B 122.5 . . ?
H4A C4 H4B 107.0 . . ?
N1 C5 C4 89(5) . . ?
N1 C5 H5A 96.5 . . ?
C4 C5 H5A 98.3 . . ?
N1 C5 H5B 135.4 . . ?
C4 C5 H5B 123.0 . . ?
H5A C5 H5B 107.5 . . ?
C5' N1' C1' 99(5) . . ?
C5' N1' H1'1 90.7 . . ?
C1' N1' H1'1 86.8 . . ?
C5' N1' H1'2 130.1 . . ?
C1' N1' H1'2 123.8 . . ?
H1'1 N1' H1'2 113.4 . . ?
C2' C1' N1' 116(7) . . ?
C2' C1' H1'3 108.4 . . ?
N1' C1' H1'3 108.4 . . ?
C2' C1' H1'4 108.4 . . ?
N1' C1' H1'4 108.4 . . ?
H1'3 C1' H1'4 107.5 . . ?
C1' C2' C3' 107(5) . . ?
C1' C2' H2'1 110.2 . . ?
C3' C2' H2'1 110.2 . . ?
C1' C2' H2'2 110.2 . . ?
C3' C2' H2'2 110.2 . . ?
H2'1 C2' H2'2 108.5 . . ?
C4' C3' C2' 108(4) . . ?
C4' C3' H3'1 110.1 . . ?
C2' C3' H3'1 110.1 . . ?
C4' C3' H3'2 110.1 . . ?
C2' C3' H3'2 110.1 . . ?
H3'1 C3' H3'2 108.5 . . ?
C5' C4' C3' 105(5) . . ?
C5' C4' H4'1 118.3 . . ?
C3' C4' H4'1 114.0 . . ?
C5' C4' H4'2 104.5 . . ?
C3' C4' H4'2 101.4 . . ?
H4'1 C4' H4'2 111.6 . . ?
C4' C5' N1' 112(5) . . ?
C4' C5' H5'1 118.0 . . ?
N1' C5' H5'1 109.8 . . ?
C4' C5' H5'2 105.8 . . ?
N1' C5' H5'2 97.1 . . ?
H5'1 C5' H5'2 112.2 . . ?

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
C5'^b H5'2^b Cl3 0.97 2.52 3.43(8) 156.0 . yes
C5'^b H5'1^b Cl1 0.97 2.96 3.57(6) 121.8 . yes
C4'^b H4'2^b Cl3 0.97 2.96 3.90(6) 164.3 6_576 yes
C4'^b H4'1^b Cl3 0.97 2.57 3.40(4) 143.8 6_566 yes
N1'^b H1'2^b Cl3 0.89 2.79 3.50(4) 138.0 1_565 yes
N1'^b H1'2^b Cl2 0.89 2.98 3.61(4) 130.1 2_665 yes
C5^a H5B^a Cl3 0.97 2.66 3.55(7) 153.5 6_576 yes
C5^a H5B^a Cl1 0.97 2.98 3.59(6) 122.2 5_676 yes
C4^a H4B^a Cl3 0.97 2.48 3.37(9) 153.2 . yes
C4^a H4A^a Cl3 0.97 2.72 3.55(6) 143.9 6_566 yes
N1^a H1B^a Cl3 0.89 2.81 3.47(8) 131.8 . yes

_refine_diff_density_max         5.332
_refine_diff_density_min         -3.450
_refine_diff_density_rms         0.383

####################################################################### 
# 
# 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_platon_tw
_database_code_depnum_ccdc_archive 'CCDC 1962914'
loop_
_audit_author_name
_audit_author_address
'chai siqian'
;Tianjin university
China
;
_audit_update_record             
;
2020-01-10 deposited with the CCDC.	2020-01-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H24 Br4 N2 Pb'
_chemical_formula_weight         699.14

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0137 0.0067 '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 0.0241 0.0134 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.9338 1.0006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -4.4950 6.8412 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 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+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   12.15(5)
_cell_length_b                   24.90(7)
_cell_length_c                   6.200(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1875(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    210(2)
_cell_measurement_reflns_used    5221
_cell_measurement_theta_min      6.30
_cell_measurement_theta_max      53.12

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.476
_exptl_crystal_F_000             1280
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    18.290
_shelx_estimated_absorpt_T_min   0.114
_shelx_estimated_absorpt_T_max   0.170
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3137
_exptl_absorpt_correction_T_max  0.7519
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      210(2)
_diffrn_radiation_wavelength     1.34139
_diffrn_radiation_type           GaK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            1531
_diffrn_reflns_av_unetI/netI     0.0634
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         3.088
_diffrn_reflns_theta_max         51.237
_diffrn_reflns_theta_full        51.237
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measured_fraction_theta_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_point_group_measured_fraction_full 0.973
_reflns_number_total             1531
_reflns_number_gt                1187
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
 Refined as a 2-component 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)+(0.1080P)²+298.2738P] 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         1531
_refine_ls_number_parameters     137
_refine_ls_number_restraints     288
_refine_ls_R_factor_all          0.1512
_refine_ls_R_factor_gt           0.1272
_refine_ls_wR_factor_ref         0.3235
_refine_ls_wR_factor_gt          0.3062
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      0.977
_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 0.62799(16) 0.250000 0.2964(3) 0.0418(7) Uani 1 2 d S T P . .
Br1 Br 0.3798(5) 0.250000 0.2470(12) 0.0684(18) Uani 1 2 d S T P . .
Br2 Br 0.6289(6) 0.250000 0.7736(8) 0.070(2) Uani 1 2 d S T P . .
Br3 Br 0.6290(5) 0.3720(2) 0.3401(10) 0.0926(19) Uani 1 1 d . . . . .
C1 C 0.882(8) 0.351(4) 0.774(13) 0.081(14) Uani 0.5 1 d D U P A 1
H1A H 0.948801 0.349071 0.863186 0.097 Uiso 0.5 1 calc R U P A 1
H1B H 0.859846 0.314191 0.739016 0.097 Uiso 0.5 1 calc R U P A 1
C2 C 0.908(9) 0.380(3) 0.572(13) 0.078(14) Uani 0.5 1 d D U P A 1
H2A H 0.841182 0.386170 0.485757 0.094 Uiso 0.5 1 calc R U P A 1
H2B H 0.961921 0.360736 0.484498 0.094 Uiso 0.5 1 calc R U P A 1
C3 C 0.953(7) 0.432(3) 0.654(18) 0.083(14) Uani 0.5 1 d D U P A 1
H3A H 1.001795 0.426236 0.778425 0.100 Uiso 0.5 1 calc R U P A 1
H3B H 0.992466 0.451659 0.541459 0.100 Uiso 0.5 1 calc R U P A 1
C4 C 0.848(8) 0.457(4) 0.714(14) 0.088(14) Uani 0.5 1 d D U P A 1
H4A H 0.854754 0.496471 0.719211 0.106 Uiso 0.5 1 calc R U P A 1
H4B H 0.788910 0.447517 0.613683 0.106 Uiso 0.5 1 calc R U P A 1
C5 C 0.828(10) 0.435(3) 0.932(13) 0.088(14) Uani 0.5 1 d D U P A 1
H5A H 0.769730 0.454733 1.005813 0.106 Uiso 0.5 1 calc R U P A 1
H5B H 0.894998 0.436119 1.018870 0.106 Uiso 0.5 1 calc R U P A 1
N1 N 0.793(7) 0.378(3) 0.896(14) 0.085(13) Uani 0.5 1 d D U P A 1
H1C H 0.782762 0.361440 1.023169 0.102 Uiso 0.5 1 calc R U P A 1
H1D H 0.730124 0.376953 0.820714 0.102 Uiso 0.5 1 calc R U P A 1
C1' C 0.860(8) 0.351(4) 0.723(12) 0.078(14) Uani 0.5 1 d D U P B 2
H1'1 H 0.871214 0.312374 0.740512 0.094 Uiso 0.5 1 calc R U P B 2
H1'2 H 0.791568 0.356899 0.642336 0.094 Uiso 0.5 1 calc R U P B 2
C2' C 0.954(7) 0.376(3) 0.608(18) 0.081(14) Uani 0.5 1 d D U P B 2
H2'1 H 0.965646 0.357895 0.468640 0.097 Uiso 0.5 1 calc R U P B 2
H2'2 H 1.021562 0.372157 0.693833 0.097 Uiso 0.5 1 calc R U P B 2
C3' C 0.925(10) 0.433(3) 0.577(13) 0.084(14) Uani 0.5 1 d D U P B 2
H3'1 H 0.986109 0.452308 0.508835 0.101 Uiso 0.5 1 calc R U P B 2
H3'2 H 0.859883 0.436304 0.484888 0.101 Uiso 0.5 1 calc R U P B 2
C4' C 0.902(8) 0.456(4) 0.794(13) 0.086(14) Uani 0.5 1 d D U P B 2
H4'1 H 0.964165 0.448349 0.891276 0.103 Uiso 0.5 1 calc R U P B 2
H4'2 H 0.891747 0.494509 0.784807 0.103 Uiso 0.5 1 calc R U P B 2
C5' C 0.801(7) 0.429(3) 0.876(19) 0.091(14) Uani 0.5 1 d D U P B 2
H5'1 H 0.745050 0.424961 0.763310 0.109 Uiso 0.5 1 calc R U P B 2
H5'2 H 0.769641 0.448145 1.000245 0.109 Uiso 0.5 1 calc R U P B 2
N1' N 0.855(7) 0.378(3) 0.936(11) 0.085(13) Uani 0.5 1 d D U P B 2
H2C H 0.922003 0.383144 0.991615 0.102 Uiso 0.5 1 calc R U P B 2
H2D H 0.813320 0.359076 1.029796 0.102 Uiso 0.5 1 calc R U P B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br2 2.958(7) . ?
Pb1 Br1 3.030(13) . ?
Pb1 Br3 3.051(10) 7_565 ?
Pb1 Br3 3.051(10) . ?
Pb1 Br1 3.072(13) 6_656 ?
C1 C2 1.48(2) . ?
C1 N1 1.48(2) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C2 C3 1.48(2) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C3 C4 1.48(2) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C4 C5 1.48(2) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C5 N1 1.49(2) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
N1 H1C 0.9000 . ?
N1 H1D 0.9000 . ?
C1' C2' 1.48(2) . ?
C1' N1' 1.48(2) . ?
C1' H1'1 0.9800 . ?
C1' H1'2 0.9800 . ?
C2' C3' 1.49(2) . ?
C2' H2'1 0.9800 . ?
C2' H2'2 0.9800 . ?
C3' C4' 1.48(2) . ?
C3' H3'1 0.9800 . ?
C3' H3'2 0.9800 . ?
C4' C5' 1.48(2) . ?
C4' H4'1 0.9800 . ?
C4' H4'2 0.9800 . ?
C5' N1' 1.49(2) . ?
C5' H5'1 0.9800 . ?
C5' H5'2 0.9800 . ?
N1' H2C 0.9000 . ?
N1' H2D 0.9000 . ?

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 Br1 96.0(2) . . ?
Br2 Pb1 Br3 84.91(13) . 7_565 ?
Br1 Pb1 Br3 90.74(12) . 7_565 ?
Br2 Pb1 Br3 84.91(13) . . ?
Br1 Pb1 Br3 90.74(12) . . ?
Br3 Pb1 Br3 169.8(3) 7_565 . ?
Br2 Pb1 Br1 94.8(2) . 6_656 ?
Br1 Pb1 Br1 169.16(8) . 6_656 ?
Br3 Pb1 Br1 90.21(12) 7_565 6_656 ?
Br3 Pb1 Br1 90.22(12) . 6_656 ?
Pb1 Br1 Pb1 179.2(3) . 6_556 ?
C2 C1 N1 111(8) . . ?
C2 C1 H1A 109.4 . . ?
N1 C1 H1A 109.4 . . ?
C2 C1 H1B 109.4 . . ?
N1 C1 H1B 109.4 . . ?
H1A C1 H1B 108.0 . . ?
C1 C2 C3 102(8) . . ?
C1 C2 H2A 111.3 . . ?
C3 C2 H2A 111.3 . . ?
C1 C2 H2B 111.3 . . ?
C3 C2 H2B 111.3 . . ?
H2A C2 H2B 109.2 . . ?
C4 C3 C2 98(8) . . ?
C4 C3 H3A 112.2 . . ?
C2 C3 H3A 112.2 . . ?
C4 C3 H3B 112.2 . . ?
C2 C3 H3B 112.2 . . ?
H3A C3 H3B 109.8 . . ?
C5 C4 C3 102(9) . . ?
C5 C4 H4A 111.4 . . ?
C3 C4 H4A 111.4 . . ?
C5 C4 H4B 111.4 . . ?
C3 C4 H4B 111.4 . . ?
H4A C4 H4B 109.2 . . ?
C4 C5 N1 106(7) . . ?
C4 C5 H5A 110.6 . . ?
N1 C5 H5A 110.6 . . ?
C4 C5 H5B 110.6 . . ?
N1 C5 H5B 110.6 . . ?
H5A C5 H5B 108.7 . . ?
C1 N1 C5 108(8) . . ?
C1 N1 H1C 110.2 . . ?
C5 N1 H1C 110.2 . . ?
C1 N1 H1D 110.2 . . ?
C5 N1 H1D 110.2 . . ?
H1C N1 H1D 108.5 . . ?
C2' C1' N1' 106(8) . . ?
C2' C1' H1'1 110.5 . . ?
N1' C1' H1'1 110.5 . . ?
C2' C1' H1'2 110.5 . . ?
N1' C1' H1'2 110.5 . . ?
H1'1 C1' H1'2 108.7 . . ?
C1' C2' C3' 106(8) . . ?
C1' C2' H2'1 110.6 . . ?
C3' C2' H2'1 110.6 . . ?
C1' C2' H2'2 110.6 . . ?
C3' C2' H2'2 110.6 . . ?
H2'1 C2' H2'2 108.7 . . ?
C4' C3' C2' 107(8) . . ?
C4' C3' H3'1 110.3 . . ?
C2' C3' H3'1 110.3 . . ?
C4' C3' H3'2 110.3 . . ?
C2' C3' H3'2 110.3 . . ?
H3'1 C3' H3'2 108.6 . . ?
C5' C4' C3' 107(9) . . ?
C5' C4' H4'1 110.2 . . ?
C3' C4' H4'1 110.2 . . ?
C5' C4' H4'2 110.2 . . ?
C3' C4' H4'2 110.2 . . ?
H4'1 C4' H4'2 108.5 . . ?
C4' C5' N1' 96(7) . . ?
C4' C5' H5'1 112.6 . . ?
N1' C5' H5'1 112.6 . . ?
C4' C5' H5'2 112.6 . . ?
N1' C5' H5'2 112.6 . . ?
H5'1 C5' H5'2 110.1 . . ?
C1' N1' C5' 101(8) . . ?
C1' N1' H2C 111.6 . . ?
C5' N1' H2C 111.6 . . ?
C1' N1' H2D 111.6 . . ?
C5' N1' H2D 111.6 . . ?
H2C N1' H2D 109.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 66(11) . . . . ?
C1 C2 C3 C4 -77(10) . . . . ?
C2 C3 C4 C5 84(9) . . . . ?
C3 C4 C5 N1 -74(11) . . . . ?
C2 C1 N1 C5 -55(11) . . . . ?
C4 C5 N1 C1 57(11) . . . . ?
N1' C1' C2' C3' -64(11) . . . . ?
C1' C2' C3' C4' 57(12) . . . . ?
C2' C3' C4' C5' -67(12) . . . . ?
C3' C4' C5' N1' 77(10) . . . . ?
C2' C1' N1' C5' 78(10) . . . . ?
C4' C5' N1' C1' -80(9) . . . . ?

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
C1^a H1A^a Br3 0.98 2.92 3.87(11) 164.9 6_657 yes
C2^a H2A^a Br3 0.98 2.75 3.68(10) 158.6 . yes
C2^a H2B^a Br3 0.98 2.87 3.71(9) 144.4 6_656 yes
N1^a H1C^a Br3 0.90 2.72 3.41(8) 133.4 1_556 yes
C1'^b H1'2^b Br3 0.98 2.75 3.71(10) 167.6 . yes
C2'^b H2'1^b Br3 0.98 2.78 3.50(9) 130.8 6_656 yes
N1'^b H2C^b Br3 0.90 2.74 3.62(9) 165.8 6_657 yes
N1'^b H2D^b Br3 0.90 2.97 3.72(8) 141.5 1_556 yes

_refine_diff_density_max         5.263
_refine_diff_density_min         -3.561
_refine_diff_density_rms         0.491

####################################################################### 
# 
# 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_pppppp
_database_code_depnum_ccdc_archive 'CCDC 1962916'
loop_
_audit_author_name
_audit_author_address
'chai siqian'
;Tianjin university
China
;
_audit_update_record             
;
2020-01-10 deposited with the CCDC.	2020-01-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C5 H12 I3 N Pb'
_chemical_formula_weight         674.05

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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   19.3160(19)
_cell_length_b                   8.2729(8)
_cell_length_c                   17.4841(17)
_cell_angle_alpha                90
_cell_angle_beta                 116.121(3)
_cell_angle_gamma                90
_cell_volume                     2508.6(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9850
_cell_measurement_theta_min      2.59
_cell_measurement_theta_max      38.75

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.569
_exptl_crystal_F_000             2320
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.210
_exptl_absorpt_coefficient_mu    20.784
_shelx_estimated_absorpt_T_min   0.068
_shelx_estimated_absorpt_T_max   0.097
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1748
_exptl_absorpt_correction_T_max  0.7477
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17269
_diffrn_reflns_av_unetI/netI     0.0777
_diffrn_reflns_av_R_equivalents  0.0969
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.098
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_full        25.100
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measured_fraction_theta_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_point_group_measured_fraction_full 0.982
_reflns_number_total             4674
_reflns_number_gt                4083
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
 Refined as a 2-component 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)+(0.3110P)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     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4674
_refine_ls_number_parameters     182
_refine_ls_number_restraints     144
_refine_ls_R_factor_all          0.1159
_refine_ls_R_factor_gt           0.1071
_refine_ls_wR_factor_ref         0.3496
_refine_ls_wR_factor_gt          0.3232
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.023
_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 1.00081(6) 0.45608(16) 0.75258(7) 0.0236(5) Uani 1 1 d . . . . .
Pb2 Pb 0.49966(6) 0.4774(2) 0.75059(7) 0.0250(5) Uani 1 1 d . . . . .
I1 I 0.85706(12) 0.6935(3) 0.66872(15) 0.0264(6) Uani 1 1 d . . . . .
I2 I 0.55524(12) 0.6839(2) 0.64156(16) 0.0258(6) Uani 1 1 d . . . . .
I3 I 1.08394(12) 0.6724(3) 0.67422(16) 0.0287(6) Uani 1 1 d . . . . .
I4 I 0.94457(12) 0.2558(3) 0.58881(15) 0.0268(6) Uani 1 1 d . . . . .
I5 I 0.41535(12) 0.2414(3) 0.59495(15) 0.0269(6) Uani 1 1 d . . . . .
I6 I 0.64421(11) 0.2374(3) 0.80640(15) 0.0272(6) Uani 1 1 d . . . . .
C10 C 0.3935(17) 0.718(4) 0.421(2) 0.020(5) Uani 1 1 d . U . . .
H10A H 0.376494 0.693023 0.360014 0.024 Uiso 1 1 calc R U . . .
H10B H 0.447146 0.678820 0.452768 0.024 Uiso 1 1 calc R U . . .
C2 C 0.8062(19) 0.898(4) 0.925(2) 0.033(5) Uani 1 1 d . U . . .
H2A H 0.807185 1.016966 0.920451 0.040 Uiso 1 1 calc R U . . .
H2B H 0.777657 0.869579 0.958503 0.040 Uiso 1 1 calc R U . . .
C1 C 0.7711(18) 0.641(4) 0.842(2) 0.030(5) Uani 1 1 d . U . . .
H1C H 0.739059 0.603660 0.869981 0.036 Uiso 1 1 calc R U . . .
H1D H 0.748829 0.596644 0.783777 0.036 Uiso 1 1 calc R U . . .
N2 N 0.8485(15) 0.580(4) 0.8892(17) 0.030(4) Uani 1 1 d . U . . .
H2C H 0.876230 0.602575 0.859663 0.036 Uiso 1 1 calc R U . . .
H2D H 0.846819 0.471145 0.893963 0.036 Uiso 1 1 calc R U . . .
C3 C 0.8889(19) 0.654(5) 0.977(2) 0.032(5) Uani 1 1 d . U . . .
H3A H 0.862787 0.620939 1.012483 0.039 Uiso 1 1 calc R U . . .
H3B H 0.943185 0.617189 1.005910 0.039 Uiso 1 1 calc R U . . .
C4 C 0.8856(19) 0.832(4) 0.967(2) 0.032(5) Uani 1 1 d . U . . .
H4A H 0.913328 0.883350 1.023397 0.038 Uiso 1 1 calc R U . . .
H4B H 0.912780 0.862740 0.932222 0.038 Uiso 1 1 calc R U . . .
C5 C 0.3119(16) 0.971(4) 0.389(2) 0.024(5) Uani 1 1 d . U . . .
H5A H 0.291809 0.958285 0.326204 0.029 Uiso 1 1 calc R U . . .
H5B H 0.315190 1.088542 0.401057 0.029 Uiso 1 1 calc R U . . .
C6 C 0.3923(17) 0.899(4) 0.4318(19) 0.024(5) Uani 1 1 d . U . . .
H6A H 0.424907 0.950202 0.407952 0.028 Uiso 1 1 calc R U . . .
H6B H 0.415085 0.924770 0.493314 0.028 Uiso 1 1 calc R U . . .
C7 C 0.3429(16) 0.629(4) 0.452(2) 0.023(5) Uani 1 1 d . U . . .
H7A H 0.364637 0.636784 0.514583 0.027 Uiso 1 1 calc R U . . .
H7B H 0.340537 0.512882 0.436441 0.027 Uiso 1 1 calc R U . . .
C8 C 0.2546(19) 0.893(4) 0.418(2) 0.031(5) Uani 1 1 d . U . . .
H8A H 0.201617 0.932014 0.381530 0.038 Uiso 1 1 calc R U . . .
H8B H 0.268447 0.922317 0.477426 0.038 Uiso 1 1 calc R U . . .
C9 C 0.7685(19) 0.821(4) 0.838(2) 0.027(5) Uani 1 1 d . U . . .
H9A H 0.714125 0.856689 0.808078 0.032 Uiso 1 1 calc R U . . .
H9B H 0.795198 0.858204 0.803734 0.032 Uiso 1 1 calc R U . . .
N1 N 0.2583(16) 0.705(3) 0.409(2) 0.031(5) Uani 1 1 d . U . . .
H1A H 0.235743 0.678794 0.352723 0.037 Uiso 1 1 calc R U . . .
H1B H 0.229908 0.657947 0.433041 0.037 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 I4 3.063(3) . ?
Pb1 I3 3.098(3) . ?
Pb1 I1 3.183(2) . ?
Pb1 I1 3.290(2) 2_746 ?
Pb1 I3 3.416(3) 2_746 ?
Pb2 I2 3.084(3) . ?
Pb2 I5 3.157(3) . ?
Pb2 I6 3.208(2) . ?
Pb2 I5 3.295(3) 2_656 ?
Pb2 I6 3.302(2) 2_656 ?
C10 C7 1.50(4) . ?
C10 C6 1.51(4) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C2 C4 1.48(4) . ?
C2 C9 1.52(5) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C1 N2 1.44(4) . ?
C1 C9 1.49(4) . ?
C1 H1C 0.9900 . ?
C1 H1D 0.9900 . ?
N2 C3 1.52(4) . ?
N2 H2C 0.9100 . ?
N2 H2D 0.9100 . ?
C3 C4 1.49(5) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.52(4) . ?
C5 C8 1.55(4) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 N1 1.60(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 N1 1.57(4) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?

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
I4 Pb1 I3 86.48(7) . . ?
I4 Pb1 I1 91.41(7) . . ?
I3 Pb1 I1 87.52(7) . . ?
I4 Pb1 I1 85.47(6) . 2_746 ?
I3 Pb1 I1 93.84(6) . 2_746 ?
I1 Pb1 I1 176.51(6) . 2_746 ?
I4 Pb1 I3 86.98(7) . 2_746 ?
I3 Pb1 I3 171.82(7) . 2_746 ?
I1 Pb1 I3 97.57(6) . 2_746 ?
I1 Pb1 I3 80.73(6) 2_746 2_746 ?
I2 Pb2 I5 89.86(7) . . ?
I2 Pb2 I6 92.16(7) . . ?
I5 Pb2 I6 85.93(7) . . ?
I2 Pb2 I5 87.47(7) . 2_656 ?
I5 Pb2 I5 176.64(8) . 2_656 ?
I6 Pb2 I5 96.20(6) . 2_656 ?
I2 Pb2 I6 85.88(7) . 2_656 ?
I5 Pb2 I6 95.54(6) . 2_656 ?
I6 Pb2 I6 177.54(8) . 2_656 ?
I5 Pb2 I6 82.23(6) 2_656 2_656 ?
Pb1 I1 Pb1 79.44(5) . 2_756 ?
Pb1 I3 Pb1 78.70(5) . 2_756 ?
Pb2 I5 Pb2 79.73(5) . 2_646 ?
Pb2 I6 Pb2 78.89(5) . 2_646 ?
C7 C10 C6 113(3) . . ?
C7 C10 H10A 108.9 . . ?
C6 C10 H10A 108.9 . . ?
C7 C10 H10B 108.9 . . ?
C6 C10 H10B 108.9 . . ?
H10A C10 H10B 107.7 . . ?
C4 C2 C9 106(3) . . ?
C4 C2 H2A 110.5 . . ?
C9 C2 H2A 110.5 . . ?
C4 C2 H2B 110.5 . . ?
C9 C2 H2B 110.5 . . ?
H2A C2 H2B 108.7 . . ?
N2 C1 C9 112(3) . . ?
N2 C1 H1C 109.1 . . ?
C9 C1 H1C 109.1 . . ?
N2 C1 H1D 109.1 . . ?
C9 C1 H1D 109.1 . . ?
H1C C1 H1D 107.9 . . ?
C1 N2 C3 112(3) . . ?
C1 N2 H2C 109.2 . . ?
C3 N2 H2C 109.2 . . ?
C1 N2 H2D 109.2 . . ?
C3 N2 H2D 109.2 . . ?
H2C N2 H2D 107.9 . . ?
C4 C3 N2 107(3) . . ?
C4 C3 H3A 110.3 . . ?
N2 C3 H3A 110.3 . . ?
C4 C3 H3B 110.3 . . ?
N2 C3 H3B 110.3 . . ?
H3A C3 H3B 108.5 . . ?
C2 C4 C3 114(3) . . ?
C2 C4 H4A 108.8 . . ?
C3 C4 H4A 108.8 . . ?
C2 C4 H4B 108.8 . . ?
C3 C4 H4B 108.8 . . ?
H4A C4 H4B 107.7 . . ?
C6 C5 C8 113(3) . . ?
C6 C5 H5A 108.9 . . ?
C8 C5 H5A 108.9 . . ?
C6 C5 H5B 108.9 . . ?
C8 C5 H5B 108.9 . . ?
H5A C5 H5B 107.7 . . ?
C10 C6 C5 113(2) . . ?
C10 C6 H6A 108.9 . . ?
C5 C6 H6A 108.9 . . ?
C10 C6 H6B 108.9 . . ?
C5 C6 H6B 108.9 . . ?
H6A C6 H6B 107.7 . . ?
C10 C7 N1 109(3) . . ?
C10 C7 H7A 109.8 . . ?
N1 C7 H7A 109.8 . . ?
C10 C7 H7B 109.8 . . ?
N1 C7 H7B 109.8 . . ?
H7A C7 H7B 108.2 . . ?
C5 C8 N1 108(3) . . ?
C5 C8 H8A 110.0 . . ?
N1 C8 H8A 110.0 . . ?
C5 C8 H8B 110.0 . . ?
N1 C8 H8B 110.0 . . ?
H8A C8 H8B 108.4 . . ?
C1 C9 C2 112(3) . . ?
C1 C9 H9A 109.2 . . ?
C2 C9 H9A 109.2 . . ?
C1 C9 H9B 109.2 . . ?
C2 C9 H9B 109.2 . . ?
H9A C9 H9B 107.9 . . ?
C8 N1 C7 115(2) . . ?
C8 N1 H1A 108.5 . . ?
C7 N1 H1A 108.5 . . ?
C8 N1 H1B 108.5 . . ?
C7 N1 H1B 108.5 . . ?
H1A N1 H1B 107.5 . . ?

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
C10 H10A I6 0.99 2.82 3.73(3) 154.1 3_666 yes
C10 H10B I2 0.99 3.03 3.75(3) 130.9 . yes
C10 H10B I5 0.99 3.18 3.84(3) 125.0 3_666 yes
N2 H2C I1 0.91 3.28 4.04(3) 142.3 . yes
N2 H2D I3 0.91 3.27 3.95(3) 132.7 2_746 yes
C3 H3A I1 0.99 3.18 3.87(4) 128.4 4_576 yes
C4 H4A I1 0.99 3.24 3.81(4) 118.8 4_576 yes
C4 H4A I3 0.99 3.22 3.95(3) 131.8 4_576 yes
C4 H4A I4 0.99 3.16 3.91(4) 134.2 4_576 yes
C4 H4B I3 0.99 3.18 3.95(4) 135.4 2_756 yes
C4 H4B I4 0.99 3.07 3.86(4) 138.2 2_756 yes
C5 H5B I5 0.99 3.33 3.96(3) 123.3 1_565 yes
C7 H7A I6 0.99 3.31 4.22(3) 153.0 2_656 yes
C7 H7B I2 0.99 3.31 4.01(3) 128.5 3_666 yes
C8 H8A I1 0.99 3.28 3.97(3) 128.1 3_676 yes
N1 H1B I4 0.91 3.30 3.95(3) 130.3 3_666 yes

_refine_diff_density_max         7.555
_refine_diff_density_min         -7.979
_refine_diff_density_rms         0.754

####################################################################### 
# 
# 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_csq-py-ysyz
_database_code_depnum_ccdc_archive 'CCDC 1962915'
loop_
_audit_author_name
_audit_author_address
'chai siqian'
;Tianjin university
China
;
_audit_update_record             
;
2020-01-10 deposited with the CCDC.	2020-01-15 downloaded from the CCDC.
;
_audit_creation_date             2019-12-23
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(Cl16 Pb4), 4(C5 H12 N)'
_chemical_formula_sum            'C20 H48 Cl8 N4 Pb2'
_chemical_formula_weight         1042.60
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'

_cell_length_a                   22.4936(8)
_cell_length_b                   23.8631(10)
_cell_length_c                   6.1802(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3317.3(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    10035
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      30.0200
_cell_measurement_theta_min      3.3690
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    10.799
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58774
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.088
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1984
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0519
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.934
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            31870
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.934
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.760
_diffrn_reflns_theta_min         2.489
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -9.00  30.00   0.50    2.11    --    0.00 -57.00 120.00   78
  2  ω    -30.00  18.00   0.50    2.11    --    0.00 -77.00-150.00   96
  3  ω    -25.00  88.00   0.50    2.11    --    0.00  57.00-150.00  226
  4  ω    -19.00   6.00   0.50    2.11    --    0.00 -77.00-120.00   50
  5  ω     37.00  64.00   0.50    2.11    --    0.00  38.00 -30.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0170277000
_diffrn_orient_matrix_UB_12      -0.0250172000
_diffrn_orient_matrix_UB_13      -0.0035790000
_diffrn_orient_matrix_UB_21      0.0265146000
_diffrn_orient_matrix_UB_22      0.0159651000
_diffrn_orient_matrix_UB_23      0.0073336000
_diffrn_orient_matrix_UB_31      -0.0011679000
_diffrn_orient_matrix_UB_32      -0.0018100000
_diffrn_orient_matrix_UB_33      0.1144795000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Mo) X-ray DW Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3861
_reflns_number_total             4528
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         1.210
_refine_diff_density_min         -1.165
_refine_diff_density_rms         0.202
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         4528
_refine_ls_number_restraints     54
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0233
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0328P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0560
_refine_ls_wR_factor_ref         0.0586
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
2. Rigid bond restraints
 N6, C7, C8, C9, C10, C2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
3. Uiso/Uaniso restraints and constraints
N6 \\sim C7 \\sim C8 \\sim C9 \\sim C10 \\sim C2: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
Uanis(N6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C1AA(H1AA,H1AB), C2(H2A,H2B), C9(H9A,H9B), N4(H4A,H4B),
 C0AA(H0AA,H0AB), C1(H1A,H1B), C5(H5A,H5B), C3(H3A,H3B), C10(H10A,H10B), C7(H7A,
 H7B), N6(H6A,H6B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb0A Pb 0.17405(2) 0.750000 0.37919(2) 0.00961(5) Uani 1 2 d S T P . .
Pb1A Pb 0.42445(2) 0.750000 0.24352(2) 0.00979(5) Uani 1 2 d S T P . .
Cl5 Cl 0.43416(3) 0.63065(3) 0.20596(12) 0.01466(15) Uani 1 1 d . . . . .
Cl4 Cl 0.39274(5) 0.750000 -0.16590(17) 0.0169(2) Uani 1 2 d S T P . .
Cl1 Cl 0.18162(5) 0.750000 0.81136(17) 0.0152(2) Uani 1 2 d S T P . .
Cl6 Cl 0.54471(4) 0.750000 0.11659(16) 0.0138(2) Uani 1 2 d S T P . .
Cl3 Cl 0.29778(4) 0.750000 0.36206(17) 0.0144(2) Uani 1 2 d S T P . .
C8 C 0.32588(17) 0.55914(16) 0.6472(6) 0.0245(8) Uani 1 1 d . U . . .
H8A H 0.359118 0.539908 0.580188 0.029 Uiso 1 1 calc R . . . .
H8B H 0.290581 0.551411 0.562057 0.029 Uiso 1 1 calc R . . . .
C1AA C 0.57085(15) 0.56621(14) 0.4858(5) 0.0176(7) Uani 1 1 d . . . . .
H1AA H 0.532004 0.557955 0.425492 0.021 Uiso 1 1 calc R . . . .
H1AB H 0.600727 0.552185 0.386408 0.021 Uiso 1 1 calc R . . . .
C2 C 0.27724(15) 0.63102(14) 0.9847(5) 0.0180(7) Uani 1 1 d . U . . .
H2A H 0.243157 0.650179 1.046089 0.022 Uiso 1 1 calc R . . . .
H2B H 0.311584 0.639233 1.074156 0.022 Uiso 1 1 calc R . . . .
C9 C 0.31711(16) 0.53705(16) 0.8771(6) 0.0226(8) Uani 1 1 d . U . . .
H9A H 0.308241 0.497281 0.872941 0.027 Uiso 1 1 calc R . . . .
H9B H 0.353251 0.542339 0.960220 0.027 Uiso 1 1 calc R . . . .
N4 N 0.54194(12) 0.62317(12) 0.8876(4) 0.0134(5) Uani 1 1 d . . . . .
H4A H 0.578067 0.630355 0.939372 0.016 Uiso 1 1 calc R . . . .
H4B H 0.515532 0.636375 0.981962 0.016 Uiso 1 1 calc R . . . .
C0AA C 0.57748(15) 0.53700(15) 0.7045(5) 0.0180(7) Uani 1 1 d . . . . .
H0AA H 0.569967 0.497211 0.687627 0.022 Uiso 1 1 calc R . . . .
H0AB H 0.617833 0.541634 0.756853 0.022 Uiso 1 1 calc R . . . .
C1 C 0.57795(14) 0.62968(14) 0.5116(5) 0.0152(6) Uani 1 1 d . . . . .
H1A H 0.618215 0.638015 0.557747 0.018 Uiso 1 1 calc R . . . .
H1B H 0.571483 0.647717 0.372978 0.018 Uiso 1 1 calc R . . . .
C5 C 0.53431(15) 0.65310(14) 0.6762(5) 0.0170(6) Uani 1 1 d . . . . .
H5A H 0.541362 0.692879 0.695887 0.020 Uiso 1 1 calc R . . . .
H5B H 0.493960 0.648188 0.624206 0.020 Uiso 1 1 calc R . . . .
C3 C 0.53423(15) 0.56132(14) 0.8680(5) 0.0183(7) Uani 1 1 d . . . . .
H3A H 0.493833 0.553074 0.823200 0.022 Uiso 1 1 calc R . . . .
H3B H 0.540760 0.543948 1.007895 0.022 Uiso 1 1 calc R . . . .
C10 C 0.26605(16) 0.56858(15) 0.9832(6) 0.0232(7) Uani 1 1 d . U . . .
H10A H 0.229515 0.560854 0.905343 0.028 Uiso 1 1 calc R . . . .
H10B H 0.261146 0.555464 1.130726 0.028 Uiso 1 1 calc R . . . .
C7 C 0.33766(15) 0.62164(15) 0.6483(6) 0.0210(7) Uani 1 1 d . U . . .
H7A H 0.374763 0.629212 0.722799 0.025 Uiso 1 1 calc R . . . .
H7B H 0.341310 0.635095 0.500813 0.025 Uiso 1 1 calc R . . . .
Cl2 Cl 0.17680(3) 0.63029(3) 0.43939(13) 0.01357(15) Uani 1 1 d . . . . .
N6 N 0.28794(12) 0.65171(12) 0.7595(4) 0.0135(5) Uani 1 1 d . U . . .
H6A H 0.254820 0.647476 0.682398 0.016 Uiso 1 1 calc R . . . .
H6B H 0.296305 0.688144 0.764217 0.016 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb0A Cl1 2.6763(11) . ?
Pb0A Cl6 2.9095(10) 6_556 ?
Pb0A Cl3 2.7851(10) . ?
Pb0A Cl2 2.8814(8) . ?
Pb0A Cl2 2.8815(8) 8_575 ?
Pb1A Cl5 2.8657(8) 8_575 ?
Pb1A Cl5 2.8658(8) . ?
Pb1A Cl4 2.6289(11) . ?
Pb1A Cl6 2.8166(10) . ?
Pb1A Cl3 2.9418(10) . ?
C8 C9 1.528(5) . ?
C8 C7 1.515(5) . ?
C1AA C0AA 1.528(5) . ?
C1AA C1 1.531(5) . ?
C2 C10 1.511(5) . ?
C2 N6 1.496(4) . ?
C9 C10 1.522(5) . ?
N4 C5 1.499(4) . ?
N4 C3 1.491(4) . ?
C0AA C3 1.518(5) . ?
C1 C5 1.520(4) . ?
C7 N6 1.496(4) . ?

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
Cl1 Pb0A Cl6 93.13(3) . 6_556 ?
Cl1 Pb0A Cl3 88.53(3) . . ?
Cl1 Pb0A Cl2 82.516(16) . 8_575 ?
Cl1 Pb0A Cl2 82.517(16) . . ?
Cl3 Pb0A Cl6 178.34(3) . 6_556 ?
Cl3 Pb0A Cl2 89.055(14) . . ?
Cl3 Pb0A Cl2 89.053(14) . 8_575 ?
Cl2 Pb0A Cl6 91.163(14) 8_575 6_556 ?
Cl2 Pb0A Cl6 91.161(14) . 6_556 ?
Cl2 Pb0A Cl2 164.96(3) . 8_575 ?
Cl5 Pb1A Cl5 167.23(3) 8_575 . ?
Cl5 Pb1A Cl3 95.395(15) 8_575 . ?
Cl5 Pb1A Cl3 95.396(15) . . ?
Cl4 Pb1A Cl5 86.717(16) . . ?
Cl4 Pb1A Cl5 86.717(16) . 8_575 ?
Cl4 Pb1A Cl6 89.57(3) . . ?
Cl4 Pb1A Cl3 88.68(3) . . ?
Cl6 Pb1A Cl5 84.503(15) . 8_575 ?
Cl6 Pb1A Cl5 84.502(15) . . ?
Cl6 Pb1A Cl3 178.25(3) . . ?
Pb1A Cl6 Pb0A 163.31(4) . 6_656 ?
Pb0A Cl3 Pb1A 167.76(4) . . ?
C7 C8 C9 111.0(3) . . ?
C0AA C1AA C1 110.4(3) . . ?
N6 C2 C10 110.3(3) . . ?
C10 C9 C8 109.1(3) . . ?
C3 N4 C5 112.8(2) . . ?
C3 C0AA C1AA 110.6(3) . . ?
C5 C1 C1AA 111.5(3) . . ?
N4 C5 C1 109.5(3) . . ?
N4 C3 C0AA 111.0(3) . . ?
C2 C10 C9 111.4(3) . . ?
N6 C7 C8 110.1(3) . . ?
C7 N6 C2 112.9(3) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.766
_oxdiff_exptl_absorpt_empirical_full_min 0.748
