# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 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_C12N4H28Pb3I12
_database_code_depnum_ccdc_archive 'CCDC 1902183'
loop_
_audit_author_name
_audit_author_address
'Xiao-Wu Lei'
;CCDC
China
;
_audit_update_record             
;
2019-03-10 deposited with the CCDC.	2019-08-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         C12N4H28Pb3I12
_chemical_formula_sum            'C12 H28 I12 N4 Pb3'
_chemical_formula_weight         2372.75

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   12.4385(10)
_cell_length_b                   11.1158(6)
_cell_length_c                   18.6465(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.358(4)
_cell_angle_gamma                90.00
_cell_volume                     2432.4(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6995
_cell_measurement_theta_min      2.5217
_cell_measurement_theta_max      27.4855

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.240
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2020
_exptl_absorpt_coefficient_mu    17.982
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.2215
_exptl_absorpt_correction_T_max  0.2665
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10999
_diffrn_reflns_av_R_equivalents  0.1018
_diffrn_reflns_av_sigmaI/netI    0.1591
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.52
_diffrn_reflns_theta_max         26.38
_reflns_number_total             4886
_reflns_number_gt                2625
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0862P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00106(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4886
_refine_ls_number_parameters     138
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0972
_refine_ls_R_factor_gt           0.0774
_refine_ls_wR_factor_ref         0.1920
_refine_ls_wR_factor_gt          0.1825
_refine_ls_goodness_of_fit_ref   0.918
_refine_ls_restrained_S_all      0.918
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.24143(6) 0.26387(7) 0.06617(4) 0.0315(3) Uani 1 1 d . . .
Pb2 Pb 0.0000 0.0000 0.0000 0.0336(3) Uani 1 2 d S . .
I6 I 0.25507(12) 0.46030(13) 0.19016(8) 0.0398(4) Uani 1 1 d . . .
I3 I 0.17359(11) 0.04442(13) 0.17192(8) 0.0373(4) Uani 1 1 d . . .
I5 I 0.50365(11) 0.19609(14) 0.13477(7) 0.0361(4) Uani 1 1 d . . .
I2 I -0.03999(12) 0.28610(14) -0.00201(10) 0.0526(5) Uani 1 1 d . . .
I4 I 0.28668(14) 0.45185(13) -0.04124(8) 0.0434(4) Uani 1 1 d . . .
I1 I 0.21075(12) 0.04369(15) -0.06229(9) 0.0463(4) Uani 1 1 d . . .
N2 N 0.4646(15) 0.3480(18) 0.3528(9) 0.041(5) Uani 1 1 d . . .
H2C H 0.4114 0.4060 0.3332 0.049 Uiso 1 1 calc R . .
N1 N 0.6163(12) 0.1900(14) 0.4009(8) 0.026(4) Uani 1 1 d . . .
H1C H 0.6725 0.1339 0.4171 0.032 Uiso 1 1 calc R . .
C5 C 0.5978(18) 0.251(2) 0.4729(12) 0.044(6) Uiso 1 1 d . . .
H5A H 0.5659 0.1941 0.4997 0.053 Uiso 1 1 calc R . .
H5B H 0.6693 0.2813 0.5076 0.053 Uiso 1 1 calc R . .
C4 C 0.5675(16) 0.365(2) 0.3272(11) 0.036(5) Uani 1 1 d . . .
H4A H 0.5424 0.3690 0.2721 0.043 Uiso 1 1 calc R . .
H4B H 0.6038 0.4415 0.3467 0.043 Uiso 1 1 calc R . .
C3 C 0.6460(19) 0.273(2) 0.3522(14) 0.044(6) Uani 1 1 d . . .
H3A H 0.7200 0.3076 0.3792 0.053 Uiso 1 1 calc R . .
H3B H 0.6522 0.2303 0.3085 0.053 Uiso 1 1 calc R . .
C2 C 0.5059(17) 0.128(2) 0.3559(11) 0.041(5) Uani 1 1 d . . .
H2A H 0.4820 0.0728 0.3882 0.049 Uiso 1 1 calc R . .
H2B H 0.5156 0.0823 0.3140 0.049 Uiso 1 1 calc R . .
C1 C 0.418(2) 0.2274(19) 0.3264(14) 0.049(6) Uani 1 1 d . . .
H1A H 0.3916 0.2261 0.2713 0.059 Uiso 1 1 calc R . .
H1B H 0.3537 0.2120 0.3431 0.059 Uiso 1 1 calc R . .
C6 C 0.5131(18) 0.356(2) 0.4400(11) 0.045(6) Uani 1 1 d . . .
H6A H 0.4512 0.3529 0.4607 0.054 Uiso 1 1 calc R . .
H6B H 0.5521 0.4326 0.4546 0.054 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
Pb1 I4 3.0726(17) . ?
Pb1 I6 3.1435(16) . ?
Pb1 I5 3.1743(15) . ?
Pb1 I2 3.3137(16) . ?
Pb1 I1 3.3566(17) . ?
Pb1 I3 3.4137(16) . ?
Pb2 I2 3.2172(16) . ?
Pb2 I2 3.2172(16) 3 ?
Pb2 I1 3.2365(15) 3 ?
Pb2 I1 3.2365(15) . ?
Pb2 I3 3.2547(14) 3 ?
Pb2 I3 3.2548(14) . ?
N2 C1 1.48(3) . ?
N2 C4 1.52(2) . ?
N2 C6 1.54(2) . ?
N2 H2C 0.9100 . ?
N1 C3 1.43(3) . ?
N1 C2 1.52(2) . ?
N1 C5 1.59(3) . ?
N1 H1C 0.9100 . ?
C5 C6 1.56(3) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C4 C3 1.39(3) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C2 C1 1.52(3) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 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
I4 Pb1 I6 91.73(4) . . ?
I4 Pb1 I5 92.20(4) . . ?
I6 Pb1 I5 94.06(4) . . ?
I4 Pb1 I2 95.61(5) . . ?
I6 Pb1 I2 91.32(4) . . ?
I5 Pb1 I2 170.39(5) . . ?
I4 Pb1 I1 91.88(4) . . ?
I6 Pb1 I1 175.52(4) . . ?
I5 Pb1 I1 88.46(4) . . ?
I2 Pb1 I1 85.69(4) . . ?
I4 Pb1 I3 174.99(4) . . ?
I6 Pb1 I3 92.00(4) . . ?
I5 Pb1 I3 90.88(4) . . ?
I2 Pb1 I3 80.96(4) . . ?
I1 Pb1 I3 84.25(4) . . ?
I2 Pb2 I2 180.0 . 3 ?
I2 Pb2 I1 90.69(4) . 3 ?
I2 Pb2 I1 89.31(4) 3 3 ?
I2 Pb2 I1 89.31(4) . . ?
I2 Pb2 I1 90.69(4) 3 . ?
I1 Pb2 I1 180.00(6) 3 . ?
I2 Pb2 I3 95.10(4) . 3 ?
I2 Pb2 I3 84.89(4) 3 3 ?
I1 Pb2 I3 88.79(4) 3 3 ?
I1 Pb2 I3 91.21(4) . 3 ?
I2 Pb2 I3 84.90(4) . . ?
I2 Pb2 I3 95.10(4) 3 . ?
I1 Pb2 I3 91.21(4) 3 . ?
I1 Pb2 I3 88.79(4) . . ?
I3 Pb2 I3 180.0 3 . ?
Pb2 I3 Pb1 75.51(3) . . ?
Pb2 I2 Pb1 77.42(3) . . ?
Pb2 I1 Pb1 76.55(3) . . ?
C1 N2 C4 106.7(17) . . ?
C1 N2 C6 112.3(18) . . ?
C4 N2 C6 104.4(15) . . ?
C1 N2 H2C 111.1 . . ?
C4 N2 H2C 111.1 . . ?
C6 N2 H2C 111.1 . . ?
C3 N1 C2 108.8(16) . . ?
C3 N1 C5 113.7(17) . . ?
C2 N1 C5 107.7(14) . . ?
C3 N1 H1C 108.9 . . ?
C2 N1 H1C 108.9 . . ?
C5 N1 H1C 108.9 . . ?
C6 C5 N1 104.9(15) . . ?
C6 C5 H5A 110.8 . . ?
N1 C5 H5A 110.8 . . ?
C6 C5 H5B 110.8 . . ?
N1 C5 H5B 110.8 . . ?
H5A C5 H5B 108.8 . . ?
C3 C4 N2 111.8(19) . . ?
C3 C4 H4A 109.2 . . ?
N2 C4 H4A 109.2 . . ?
C3 C4 H4B 109.2 . . ?
N2 C4 H4B 109.2 . . ?
H4A C4 H4B 107.9 . . ?
C4 C3 N1 113.0(19) . . ?
C4 C3 H3A 109.0 . . ?
N1 C3 H3A 109.0 . . ?
C4 C3 H3B 109.0 . . ?
N1 C3 H3B 109.0 . . ?
H3A C3 H3B 107.8 . . ?
N1 C2 C1 105.8(18) . . ?
N1 C2 H2A 110.6 . . ?
C1 C2 H2A 110.6 . . ?
N1 C2 H2B 110.6 . . ?
C1 C2 H2B 110.6 . . ?
H2A C2 H2B 108.7 . . ?
N2 C1 C2 112.9(19) . . ?
N2 C1 H1A 109.0 . . ?
C2 C1 H1A 109.0 . . ?
N2 C1 H1B 109.0 . . ?
C2 C1 H1B 109.0 . . ?
H1A C1 H1B 107.8 . . ?
N2 C6 C5 110.4(17) . . ?
N2 C6 H6A 109.6 . . ?
C5 C6 H6A 109.6 . . ?
N2 C6 H6B 109.6 . . ?
C5 C6 H6B 109.6 . . ?
H6A C6 H6B 108.1 . . ?

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.178 0.250 -0.038 143.2 29.5
2 0.822 0.750 0.038 143.3 28.7
3 0.322 0.750 0.462 143.2 28.0
4 0.678 0.250 0.538 143.3 30.1

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        26.38
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         3.668
_refine_diff_density_min         -3.892
_refine_diff_density_rms         0.551
####################################################################### 
# 
# 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_C14N6H38Pb3Br10
_database_code_depnum_ccdc_archive 'CCDC 1902193'
loop_
_audit_author_name
_audit_author_address
'Xiao-Wu Lei'
;CCDC
China
;
_audit_update_record             
;
2019-03-10 deposited with the CCDC.	2019-08-09 downloaded from the CCDC.
;
#================================================ 

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         C14N6H38Pb3Br10
_chemical_formula_sum            'C14 H38 Br10 N6 Pb3'
_chemical_formula_weight         1711.17

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   11.270(3)
_cell_length_b                   15.861(4)
_cell_length_c                   11.479(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 118.201(3)
_cell_angle_gamma                90.00
_cell_volume                     1808.2(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7358
_cell_measurement_theta_min      2.19
_cell_measurement_theta_max      28.23

_exptl_crystal_description       block
_exptl_crystal_colour            'light yellow'
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.143
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1520
_exptl_absorpt_coefficient_mu    24.997
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0821
_exptl_absorpt_correction_T_max  0.1173
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6832
_diffrn_reflns_av_R_equivalents  0.0608
_diffrn_reflns_av_sigmaI/netI    0.0978
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.26
_diffrn_reflns_theta_max         26.05
_reflns_number_total             3386
_reflns_number_gt                2322
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0555P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00284(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3386
_refine_ls_number_parameters     152
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0676
_refine_ls_R_factor_gt           0.0578
_refine_ls_wR_factor_ref         0.1350
_refine_ls_wR_factor_gt          0.1334
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.020
_refine_ls_shift/su_max          0.004
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.30147(5) 0.01144(4) 0.36685(5) 0.0286(2) Uani 1 1 d . . .
Pb2 Pb 0.0000 0.0000 0.0000 0.0273(2) Uani 1 2 d S . .
Br1 Br 0.54269(14) 0.13381(9) 0.45543(14) 0.0297(4) Uani 1 1 d . . .
Br2 Br 0.04246(16) -0.08928(10) 0.25140(15) 0.0371(4) Uani 1 1 d . . .
Br3 Br 0.11334(15) 0.14942(9) 0.18798(14) 0.0310(4) Uani 1 1 d . . .
Br4 Br 0.29015(18) 0.07644(11) 0.59409(16) 0.0422(5) Uani 1 1 d . . .
Br5 Br 0.29425(16) -0.03662(11) 0.09635(16) 0.0407(5) Uani 1 1 d . . .
N3 N 0.9448(9) 0.3081(6) 0.9121(10) 0.016(2) Uani 1 1 d . . .
H3A H 1.0194 0.3051 0.9910 0.020 Uiso 1 1 calc . . .
H3B H 0.9631 0.2843 0.8511 0.020 Uiso 1 1 calc . . .
N1 N 0.1928(12) 0.2679(7) 0.4567(11) 0.031(3) Uani 1 1 d . . .
H1A H 0.1234 0.2708 0.3756 0.046 Uiso 1 1 calc . . .
H1B H 0.1701 0.2915 0.5138 0.046 Uiso 1 1 calc . . .
H1C H 0.2147 0.2142 0.4785 0.046 Uiso 1 1 calc . . .
N2 N 0.6713(10) 0.3517(7) 0.7433(11) 0.021(3) Uani 1 1 d . . .
C7 C 0.3094(14) 0.3135(9) 0.4605(13) 0.027(3) Uani 1 1 d . . .
H7A H 0.2851 0.3717 0.4347 0.032 Uiso 1 1 calc . . .
H7B H 0.3344 0.2879 0.3984 0.032 Uiso 1 1 calc . . .
C6 C 0.4273(14) 0.3099(9) 0.5984(14) 0.025(3) Uani 1 1 d . . .
H6A H 0.4509 0.2515 0.6239 0.030 Uiso 1 1 calc . . .
H6B H 0.4016 0.3352 0.6601 0.030 Uiso 1 1 calc . . .
C5 C 0.7850(13) 0.3998(9) 0.7442(14) 0.025(3) Uani 1 1 d . . .
H5A H 0.7599 0.4586 0.7242 0.030 Uiso 1 1 calc . . .
H5B H 0.8055 0.3777 0.6770 0.030 Uiso 1 1 calc . . .
C4 C 0.5494(14) 0.3564(9) 0.6056(13) 0.027(3) Uani 1 1 d . . .
H4A H 0.5730 0.3321 0.5418 0.033 Uiso 1 1 calc . . .
H4B H 0.5259 0.4151 0.5821 0.033 Uiso 1 1 calc . . .
C3 C 0.9081(14) 0.3926(11) 0.8790(15) 0.038(4) Uani 1 1 d . . .
H3C H 0.9825 0.4231 0.8785 0.046 Uiso 1 1 calc . . .
H3D H 0.8890 0.4181 0.9452 0.046 Uiso 1 1 calc . . .
C2 C 0.8393(14) 0.2641(10) 0.9176(15) 0.034(4) Uani 1 1 d . . .
H2A H 0.8202 0.2901 0.9834 0.040 Uiso 1 1 calc . . .
H2B H 0.8675 0.2065 0.9451 0.040 Uiso 1 1 calc . . .
C1 C 0.7121(14) 0.2634(9) 0.7855(14) 0.029(4) Uani 1 1 d . . .
H1D H 0.7284 0.2342 0.7202 0.035 Uiso 1 1 calc . . .
H1E H 0.6408 0.2342 0.7938 0.035 Uiso 1 1 calc . . .


_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 Br4 2.8631(19) . ?
Pb1 Br1 3.0278(16) 3_656 ?
Pb1 Br2 3.0286(17) . ?
Pb1 Br3 3.0637(16) . ?
Pb1 Br1 3.0949(17) . ?
Pb1 Br5 3.1607(19) . ?
Pb2 Br5 3.0151(18) . ?
Pb2 Br5 3.0151(18) 3 ?
Pb2 Br2 3.0425(17) . ?
Pb2 Br2 3.0426(17) 3 ?
Pb2 Br3 3.0495(16) . ?
Pb2 Br3 3.0495(16) 3 ?
Br1 Pb1 3.0278(16) 3_656 ?
N3 C3 1.402(19) . ?
N3 C2 1.405(18) . ?
N3 H3A 0.9000 . ?
N3 H3B 0.9000 . ?
N1 C7 1.482(18) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N2 C1 1.482(17) . ?
N2 C5 1.487(16) . ?
N2 C4 1.529(16) . ?
C7 C6 1.512(18) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C6 C4 1.529(19) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C5 C3 1.52(2) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C3 H3C 0.9700 . ?
C3 H3D 0.9700 . ?
C2 C1 1.516(19) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C1 H1D 0.9700 . ?
C1 H1E 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
Br4 Pb1 Br1 85.50(5) . 3_656 ?
Br4 Pb1 Br2 98.04(5) . . ?
Br1 Pb1 Br2 91.47(5) 3_656 . ?
Br4 Pb1 Br3 92.22(5) . . ?
Br1 Pb1 Br3 172.96(5) 3_656 . ?
Br2 Pb1 Br3 82.24(5) . . ?
Br4 Pb1 Br1 83.41(5) . . ?
Br1 Pb1 Br1 96.66(4) 3_656 . ?
Br2 Pb1 Br1 171.83(5) . . ?
Br3 Pb1 Br1 89.68(5) . . ?
Br4 Pb1 Br5 172.01(5) . . ?
Br1 Pb1 Br5 102.46(5) 3_656 . ?
Br2 Pb1 Br5 82.58(4) . . ?
Br3 Pb1 Br5 79.95(5) . . ?
Br1 Pb1 Br5 94.86(5) . . ?
Br5 Pb2 Br5 180.0 . 3 ?
Br5 Pb2 Br2 84.82(4) . . ?
Br5 Pb2 Br2 95.18(4) 3 . ?
Br5 Pb2 Br2 95.18(4) . 3 ?
Br5 Pb2 Br2 84.82(4) 3 3 ?
Br2 Pb2 Br2 180.0 . 3 ?
Br5 Pb2 Br3 82.52(4) . . ?
Br5 Pb2 Br3 97.48(4) 3 . ?
Br2 Pb2 Br3 82.25(4) . . ?
Br2 Pb2 Br3 97.75(4) 3 . ?
Br5 Pb2 Br3 97.48(4) . 3 ?
Br5 Pb2 Br3 82.52(4) 3 3 ?
Br2 Pb2 Br3 97.75(4) . 3 ?
Br2 Pb2 Br3 82.25(4) 3 3 ?
Br3 Pb2 Br3 180.0 . 3 ?
Pb1 Br1 Pb1 83.34(4) 3_656 . ?
Pb1 Br2 Pb2 81.75(4) . . ?
Pb2 Br3 Pb1 81.07(4) . . ?
Pb2 Br5 Pb1 80.05(4) . . ?
C3 N3 C2 109.8(10) . . ?
C3 N3 H3A 109.7 . . ?
C2 N3 H3A 109.7 . . ?
C3 N3 H3B 109.7 . . ?
C2 N3 H3B 109.7 . . ?
H3A N3 H3B 108.2 . . ?
C7 N1 H1A 109.5 . . ?
C7 N1 H1B 109.5 . . ?
H1A N1 H1B 109.5 . . ?
C7 N1 H1C 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N2 C5 110.5(10) . . ?
C1 N2 C4 111.8(10) . . ?
C5 N2 C4 109.4(10) . . ?
N1 C7 C6 109.9(11) . . ?
N1 C7 H7A 109.7 . . ?
C6 C7 H7A 109.7 . . ?
N1 C7 H7B 109.7 . . ?
C6 C7 H7B 109.7 . . ?
H7A C7 H7B 108.2 . . ?
C7 C6 C4 111.2(12) . . ?
C7 C6 H6A 109.4 . . ?
C4 C6 H6A 109.4 . . ?
C7 C6 H6B 109.4 . . ?
C4 C6 H6B 109.4 . . ?
H6A C6 H6B 108.0 . . ?
N2 C5 C3 109.7(11) . . ?
N2 C5 H5A 109.7 . . ?
C3 C5 H5A 109.7 . . ?
N2 C5 H5B 109.7 . . ?
C3 C5 H5B 109.7 . . ?
H5A C5 H5B 108.2 . . ?
N2 C4 C6 112.3(11) . . ?
N2 C4 H4A 109.1 . . ?
C6 C4 H4A 109.1 . . ?
N2 C4 H4B 109.1 . . ?
C6 C4 H4B 109.1 . . ?
H4A C4 H4B 107.9 . . ?
N3 C3 C5 111.0(12) . . ?
N3 C3 H3C 109.4 . . ?
C5 C3 H3C 109.4 . . ?
N3 C3 H3D 109.4 . . ?
C5 C3 H3D 109.4 . . ?
H3C C3 H3D 108.0 . . ?
N3 C2 C1 112.2(12) . . ?
N3 C2 H2A 109.2 . . ?
C1 C2 H2A 109.2 . . ?
N3 C2 H2B 109.2 . . ?
C1 C2 H2B 109.2 . . ?
H2A C2 H2B 107.9 . . ?
N2 C1 C2 108.7(11) . . ?
N2 C1 H1D 109.9 . . ?
C2 C1 H1D 109.9 . . ?
N2 C1 H1E 109.9 . . ?
C2 C1 H1E 109.9 . . ?
H1D C1 H1E 108.3 . . ?

_diffrn_measured_fraction_theta_max 0.948
_diffrn_reflns_theta_full        26.05
_diffrn_measured_fraction_theta_full 0.948
_refine_diff_density_max         4.417
_refine_diff_density_min         -3.935
_refine_diff_density_rms         0.455
####################################################################### 
# 
# 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_C16N4H44Pb3I10
_database_code_depnum_ccdc_archive 'CCDC 1902184'
loop_
_audit_author_name
_audit_author_address
'Xiao-Wu Lei'
;CCDC
China
;
_audit_update_record             
;
2019-03-10 deposited with the CCDC.	2019-08-09 downloaded from the CCDC.
;
#================================================

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         C16N4H44Pb3I10
_chemical_formula_sum            'C16 H44 I10 N4 Pb3'
_chemical_formula_weight         2183.12

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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.5123(8)
_cell_length_b                   13.4417(12)
_cell_length_c                   19.1192(17)
_cell_angle_alpha                75.6650(10)
_cell_angle_beta                 89.9240(10)
_cell_angle_gamma                72.4660(10)
_cell_volume                     2251.3(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    8288
_cell_measurement_theta_min      2.21
_cell_measurement_theta_max      27.19

_exptl_crystal_description       block
_exptl_crystal_colour            light
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.220
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1888
_exptl_absorpt_coefficient_mu    18.059
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3260
_exptl_absorpt_correction_T_max  0.3260
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26362
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_sigmaI/netI    0.0467
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.65
_diffrn_reflns_theta_max         27.56
_reflns_number_total             10146
_reflns_number_gt                8128
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0335P)²+7.0660P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10146
_refine_ls_number_parameters     301
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0366
_refine_ls_wR_factor_ref         0.0872
_refine_ls_wR_factor_gt          0.0824
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.80650(3) 0.86670(3) 0.101029(18) 0.03642(9) Uani 1 1 d . . .
Pb2 Pb 0.85047(3) 0.76794(3) 0.330163(18) 0.03628(9) Uani 1 1 d . . .
Pb3 Pb 0.93409(4) 0.53168(3) 0.206063(19) 0.03747(9) Uani 1 1 d . . .
I11 I 0.62225(6) 0.74516(5) 0.20876(3) 0.03665(13) Uani 1 1 d . . .
I10 I 1.09638(6) 0.72024(4) 0.20453(3) 0.03706(13) Uani 1 1 d . . .
I9 I 0.78047(7) 1.01482(5) 0.21638(4) 0.04914(16) Uani 1 1 d . . .
I8 I 0.85737(7) 0.65307(6) 0.03626(3) 0.04944(16) Uani 1 1 d . . .
I7 I 1.10497(7) 0.78195(5) 0.42610(4) 0.04696(15) Uani 1 1 d . . .
I6 I 0.91591(6) 0.51327(5) 0.38331(4) 0.04594(15) Uani 1 1 d . . .
I5 I 0.77207(7) 0.36325(5) 0.21149(4) 0.05093(16) Uani 1 1 d . . .
I4 I 1.0000 1.0000 0.0000 0.0629(3) Uani 1 2 d S . .
I3 I 0.5000 1.0000 0.0000 0.0552(2) Uani 1 2 d S . .
I2 I 1.25717(7) 0.39047(5) 0.20064(4) 0.05443(18) Uani 1 1 d . . .
I1 I 0.58558(7) 0.82543(6) 0.42216(4) 0.05605(18) Uani 1 1 d . . .
N4 N 1.2267(8) 0.0623(6) 0.2057(4) 0.0386(17) Uani 1 1 d . . .
C15 C 1.1470(12) 0.1139(10) 0.2621(6) 0.062(3) Uani 1 1 d . . .
H15A H 1.1480 0.1880 0.2517 0.074 Uiso 1 1 calc R . .
H15B H 1.0447 0.1152 0.2592 0.074 Uiso 1 1 calc R . .
C14 C 1.3871(10) 0.0614(10) 0.2063(6) 0.058(3) Uani 1 1 d . . .
H14A H 1.4399 0.0141 0.2508 0.070 Uiso 1 1 calc R . .
H14B H 1.3908 0.1332 0.2022 0.070 Uiso 1 1 calc R . .
H14C H 1.4317 0.0364 0.1662 0.070 Uiso 1 1 calc R . .
C13 C 1.2236(12) -0.0492(8) 0.2106(7) 0.066(3) Uani 1 1 d . . .
H13A H 1.1229 -0.0499 0.2103 0.080 Uiso 1 1 calc R . .
H13B H 1.2774 -0.0971 0.2547 0.080 Uiso 1 1 calc R . .
H13C H 1.2682 -0.0725 0.1700 0.080 Uiso 1 1 calc R . .
N3 N 1.1333(10) 0.1116(7) 0.3927(5) 0.057(2) Uani 1 1 d . . .
C12 C 1.2135(12) 0.0568(10) 0.3361(6) 0.064(3) Uani 1 1 d . . .
H12A H 1.3164 0.0542 0.3389 0.077 Uiso 1 1 calc R . .
H12B H 1.2105 -0.0169 0.3471 0.077 Uiso 1 1 calc R . .
N2 N 0.3930(7) 0.6444(6) 0.0055(4) 0.0398(17) Uani 1 1 d . . .
C4 C 0.3080(10) 0.4681(9) 0.4128(6) 0.055(3) Uani 1 1 d . . .
H4A H 0.2446 0.5347 0.4202 0.066 Uiso 1 1 calc R . .
H4B H 0.3041 0.4092 0.4523 0.066 Uiso 1 1 calc R . .
H4C H 0.2757 0.4580 0.3683 0.066 Uiso 1 1 calc R . .
C16 C 0.9721(12) 0.1146(10) 0.3904(7) 0.067(3) Uani 1 1 d . . .
H16A H 0.9669 0.0434 0.3936 0.101 Uiso 1 1 calc R . .
H16B H 0.9211 0.1630 0.3459 0.101 Uiso 1 1 calc R . .
H16C H 0.9267 0.1393 0.4305 0.101 Uiso 1 1 calc R . .
C8 C 0.2351(11) 0.6433(11) 0.0036(7) 0.073(4) Uani 1 1 d . . .
H8A H 0.1741 0.7026 0.0203 0.087 Uiso 1 1 calc R . .
H8B H 0.2295 0.5765 0.0344 0.087 Uiso 1 1 calc R . .
H8C H 0.2011 0.6501 -0.0451 0.087 Uiso 1 1 calc R . .
C11 C 1.1481(13) 0.1373(9) 0.1359(6) 0.067(3) Uani 1 1 d . . .
H11A H 1.0464 0.1393 0.1342 0.080 Uiso 1 1 calc R . .
H11B H 1.1941 0.1121 0.0961 0.080 Uiso 1 1 calc R . .
H11C H 1.1534 0.2085 0.1326 0.080 Uiso 1 1 calc R . .
C7 C 0.4366(12) 0.6496(11) 0.0775(6) 0.071(3) Uani 1 1 d . . .
H7A H 0.3654 0.7087 0.0903 0.085 Uiso 1 1 calc R . .
H7B H 0.5321 0.6601 0.0774 0.085 Uiso 1 1 calc R . .
H7C H 0.4411 0.5833 0.1123 0.085 Uiso 1 1 calc R . .
C10 C 1.2109(15) 0.0388(9) 0.4629(7) 0.075(4) Uani 1 1 d . . .
H10A H 1.2047 -0.0325 0.4675 0.112 Uiso 1 1 calc R . .
H10B H 1.1651 0.0659 0.5021 0.112 Uiso 1 1 calc R . .
H10C H 1.3129 0.0361 0.4643 0.112 Uiso 1 1 calc R . .
C3 C 0.4703(13) 0.5598(10) 0.3446(7) 0.078(4) Uani 1 1 d . . .
H3A H 0.5697 0.5630 0.3417 0.093 Uiso 1 1 calc R . .
H3B H 0.4056 0.6278 0.3491 0.093 Uiso 1 1 calc R . .
H3C H 0.4395 0.5451 0.3015 0.093 Uiso 1 1 calc R . .
C2 C 0.5669(13) 0.3678(10) 0.3982(8) 0.083(4) Uani 1 1 d . . .
H2A H 0.6660 0.3718 0.3960 0.100 Uiso 1 1 calc R . .
H2B H 0.5361 0.3567 0.3537 0.100 Uiso 1 1 calc R . .
H2C H 0.5640 0.3087 0.4378 0.100 Uiso 1 1 calc R . .
C6 C 0.3991(14) 0.7423(10) -0.0494(7) 0.078(4) Uani 1 1 d . . .
H6A H 0.3348 0.8054 -0.0379 0.094 Uiso 1 1 calc R . .
H6B H 0.3677 0.7394 -0.0964 0.094 Uiso 1 1 calc R . .
H6C H 0.4986 0.7453 -0.0495 0.094 Uiso 1 1 calc R . .
C9 C 1.1438(18) 0.2181(10) 0.3888(7) 0.089(4) Uani 1 1 d . . .
H9A H 1.0945 0.2671 0.3441 0.133 Uiso 1 1 calc R . .
H9B H 1.2460 0.2147 0.3910 0.133 Uiso 1 1 calc R . .
H9C H 1.0979 0.2429 0.4287 0.133 Uiso 1 1 calc R . .
C5 C 0.4992(14) 0.5516(10) -0.0190(8) 0.078(4) Uani 1 1 d . . .
H5A H 0.4736 0.5610 -0.0699 0.094 Uiso 1 1 calc . . .
H5B H 0.5984 0.5565 -0.0149 0.094 Uiso 1 1 calc . . .
N1 N 0.4642(8) 0.4721(7) 0.4092(4) 0.0451(19) Uani 1 1 d . . .
C1 C 0.515(2) 0.495(3) 0.4732(11) 0.217(15) Uani 1 1 d D . .
H1A H 0.6108 0.4391 0.4855 0.260 Uiso 1 1 calc . . .
H1B H 0.5388 0.5606 0.4521 0.260 Uiso 1 1 calc . . .


_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 I11 3.1673(6) . ?
Pb1 I10 3.1952(7) . ?
Pb1 I4 3.2548(4) . ?
Pb1 I3 3.2550(4) . ?
Pb1 I9 3.2811(8) . ?
Pb1 I8 3.3069(8) . ?
Pb2 I1 3.0867(8) . ?
Pb2 I7 3.1173(7) . ?
Pb2 I6 3.1834(8) . ?
Pb2 I11 3.3106(7) . ?
Pb2 I9 3.3594(8) . ?
Pb2 I10 3.3906(7) . ?
Pb3 I5 3.0818(7) . ?
Pb3 I2 3.1048(8) . ?
Pb3 I8 3.2250(8) . ?
Pb3 I10 3.3360(7) . ?
Pb3 I6 3.3444(8) . ?
I4 Pb1 3.2548(4) 2_775 ?
I3 Pb1 3.2550(4) 2_675 ?
N4 C13 1.488(12) . ?
N4 C11 1.496(13) . ?
N4 C15 1.507(12) . ?
N4 C14 1.522(11) . ?
C15 C12 1.471(15) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
N3 C9 1.448(14) . ?
N3 C10 1.490(14) . ?
N3 C16 1.522(14) . ?
N3 C12 1.532(13) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
N2 C7 1.464(13) . ?
N2 C6 1.482(13) . ?
N2 C8 1.507(11) . ?
N2 C5 1.524(14) . ?
C4 N1 1.503(11) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C3 N1 1.496(13) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C2 N1 1.511(14) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C5 C5 1.39(3) 2_665 ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
N1 C1 1.450(15) . ?
C1 C1 1.10(3) 2_666 ?
C1 H1A 0.9700 . ?
C1 H1B 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
I11 Pb1 I10 88.074(17) . . ?
I11 Pb1 I4 175.630(16) . . ?
I10 Pb1 I4 90.332(14) . . ?
I11 Pb1 I3 87.863(14) . . ?
I10 Pb1 I3 175.380(15) . . ?
I4 Pb1 I3 93.876(10) . . ?
I11 Pb1 I9 84.967(18) . . ?
I10 Pb1 I9 81.935(18) . . ?
I4 Pb1 I9 90.782(15) . . ?
I3 Pb1 I9 99.893(15) . . ?
I11 Pb1 I8 81.151(18) . . ?
I10 Pb1 I8 84.255(18) . . ?
I4 Pb1 I8 102.742(15) . . ?
I3 Pb1 I8 92.945(15) . . ?
I9 Pb1 I8 160.70(2) . . ?
I1 Pb2 I7 101.24(2) . . ?
I1 Pb2 I6 95.73(2) . . ?
I7 Pb2 I6 97.164(19) . . ?
I1 Pb2 I11 88.30(2) . . ?
I7 Pb2 I11 170.442(19) . . ?
I6 Pb2 I11 82.338(17) . . ?
I1 Pb2 I9 96.78(2) . . ?
I7 Pb2 I9 96.568(19) . . ?
I6 Pb2 I9 159.24(2) . . ?
I11 Pb2 I9 81.541(17) . . ?
I1 Pb2 I10 170.04(2) . . ?
I7 Pb2 I10 87.852(18) . . ?
I6 Pb2 I10 87.063(17) . . ?
I11 Pb2 I10 82.590(17) . . ?
I9 Pb2 I10 77.968(17) . . ?
I5 Pb3 I2 99.96(2) . . ?
I5 Pb3 I8 97.50(2) . . ?
I2 Pb3 I8 99.22(2) . . ?
I5 Pb3 I10 177.20(2) . . ?
I2 Pb3 I10 82.518(18) . . ?
I8 Pb3 I10 83.328(18) . . ?
I5 Pb3 I6 92.790(19) . . ?
I2 Pb3 I6 101.76(2) . . ?
I8 Pb3 I6 154.62(2) . . ?
I10 Pb3 I6 85.400(16) . . ?
Pb1 I11 Pb2 81.575(16) . . ?
Pb1 I10 Pb3 81.045(16) . . ?
Pb1 I10 Pb2 79.937(16) . . ?
Pb3 I10 Pb2 79.627(15) . . ?
Pb1 I9 Pb2 79.198(17) . . ?
Pb3 I8 Pb1 81.056(18) . . ?
Pb2 I6 Pb3 82.535(17) . . ?
Pb1 I4 Pb1 180.0 . 2_775 ?
Pb1 I3 Pb1 179.999(11) 2_675 . ?
C13 N4 C11 110.1(8) . . ?
C13 N4 C15 115.5(8) . . ?
C11 N4 C15 103.3(8) . . ?
C13 N4 C14 108.5(8) . . ?
C11 N4 C14 107.8(8) . . ?
C15 N4 C14 111.2(7) . . ?
C12 C15 N4 112.8(9) . . ?
C12 C15 H15A 109.0 . . ?
N4 C15 H15A 109.0 . . ?
C12 C15 H15B 109.0 . . ?
N4 C15 H15B 109.0 . . ?
H15A C15 H15B 107.8 . . ?
N4 C14 H14A 109.5 . . ?
N4 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N4 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N4 C13 H13A 109.5 . . ?
N4 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N4 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C9 N3 C10 107.3(9) . . ?
C9 N3 C16 110.4(10) . . ?
C10 N3 C16 109.2(9) . . ?
C9 N3 C12 115.6(10) . . ?
C10 N3 C12 103.7(9) . . ?
C16 N3 C12 110.2(8) . . ?
C15 C12 N3 112.2(9) . . ?
C15 C12 H12A 109.2 . . ?
N3 C12 H12A 109.2 . . ?
C15 C12 H12B 109.2 . . ?
N3 C12 H12B 109.2 . . ?
H12A C12 H12B 107.9 . . ?
C7 N2 C6 109.8(9) . . ?
C7 N2 C8 108.9(8) . . ?
C6 N2 C8 107.4(9) . . ?
C7 N2 C5 113.2(9) . . ?
C6 N2 C5 103.9(9) . . ?
C8 N2 C5 113.3(8) . . ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N3 C16 H16A 109.5 . . ?
N3 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
N3 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N2 C8 H8A 109.5 . . ?
N2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N4 C11 H11A 109.5 . . ?
N4 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N4 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N2 C7 H7A 109.5 . . ?
N2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N3 C10 H10A 109.5 . . ?
N3 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N3 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C3 H3A 109.5 . . ?
N1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N2 C6 H6A 109.5 . . ?
N2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N3 C9 H9A 109.5 . . ?
N3 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N3 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C5 C5 N2 115.5(14) 2_665 . ?
C5 C5 H5A 108.4 2_665 . ?
N2 C5 H5A 108.4 . . ?
C5 C5 H5B 108.4 2_665 . ?
N2 C5 H5B 108.4 . . ?
H5A C5 H5B 107.5 . . ?
C1 N1 C3 108.4(15) . . ?
C1 N1 C4 111.8(9) . . ?
C3 N1 C4 108.8(8) . . ?
C1 N1 C2 110.3(15) . . ?
C3 N1 C2 106.7(9) . . ?
C4 N1 C2 110.7(8) . . ?
C1 C1 N1 143(2) 2_666 . ?
C1 C1 H1A 101.2 2_666 . ?
N1 C1 H1A 101.2 . . ?
C1 C1 H1B 101.2 2_666 . ?
N1 C1 H1B 101.2 . . ?
H1A C1 H1B 104.5 . . ?

_diffrn_measured_fraction_theta_max 0.973
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.973
_refine_diff_density_max         2.832
_refine_diff_density_min         -1.134
_refine_diff_density_rms         0.205
####################################################################### 
# 
# 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_C8N2H21Pb3I9
_database_code_depnum_ccdc_archive 'CCDC 1902195'
loop_
_audit_author_name
_audit_author_address
'Xiao-Wu Lei'
;CCDC
China
;
_audit_update_record             
;
2019-03-10 deposited with the CCDC.	2019-08-09 downloaded from the CCDC.
;
#================================================

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         C8N2H21Pb3I9
_chemical_formula_sum            'C8 H21 I9 N2 Pb3'
_chemical_formula_weight         1908.94

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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pnma

loop_
_symmetry_equiv_pos_as_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                   24.171(6)
_cell_length_b                   15.841(4)
_cell_length_c                   9.290(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3557.1(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8921
_cell_measurement_theta_min      2.1187
_cell_measurement_theta_max      25.0218

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.565
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3224
_exptl_absorpt_coefficient_mu    21.975
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2173
_exptl_absorpt_correction_T_max  0.2724
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17566
_diffrn_reflns_av_R_equivalents  0.0930
_diffrn_reflns_av_sigmaI/netI    0.0765
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.12
_diffrn_reflns_theta_max         25.03
_reflns_number_total             3229
_reflns_number_gt                2489
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0304P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00022(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3229
_refine_ls_number_parameters     110
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_gt           0.0379
_refine_ls_wR_factor_ref         0.0858
_refine_ls_wR_factor_gt          0.0839
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_restrained_S_all      1.003
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.292239(17) 0.11942(2) 0.46102(4) 0.03608(15) Uani 1 1 d . . .
Pb2 Pb 0.44513(2) 0.2500 0.47406(6) 0.03877(18) Uani 1 2 d S . .
I7 I 0.34014(4) 0.2500 0.22399(10) 0.0413(3) Uani 1 2 d S . .
I6 I 0.41686(3) 0.04775(4) 0.46643(7) 0.0451(2) Uani 1 1 d . . .
I5 I 0.33647(4) 0.2500 0.70824(10) 0.0425(3) Uani 1 2 d S . .
I4 I 0.53293(5) 0.2500 0.23890(13) 0.0617(3) Uani 1 2 d S . .
I3 I 0.52455(5) 0.2500 0.72931(13) 0.0618(3) Uani 1 2 d S . .
I2 I 0.18808(5) 0.2500 0.45879(18) 0.0798(5) Uani 1 2 d S . .
I1 I 0.26065(4) 0.00024(5) 0.19870(10) 0.0739(3) Uani 1 1 d . . .
N1 N 0.4419(4) 0.0150(5) 0.9564(8) 0.038(2) Uani 1 1 d . . .
C4 C 0.4881(4) 0.0124(7) 0.8504(11) 0.048(3) Uani 1 1 d . . .
H4A H 0.4797 0.0487 0.7693 0.058 Uiso 1 1 calc . . .
H4B H 0.4929 -0.0447 0.8149 0.058 Uiso 1 1 calc . . .
C3 C 0.4249(7) 0.1003(8) 1.0005(17) 0.087(5) Uani 1 1 d . . .
H3A H 0.4137 0.1320 0.9173 0.130 Uiso 1 1 calc . . .
H3B H 0.4554 0.1283 1.0464 0.130 Uiso 1 1 calc . . .
H3C H 0.3945 0.0965 1.0667 0.130 Uiso 1 1 calc . . .
C2 C 0.4585(6) -0.0422(8) 1.0757(13) 0.068(4) Uani 1 1 d . . .
H2A H 0.4640 -0.0987 1.0380 0.082 Uiso 1 1 calc . . .
H2B H 0.4289 -0.0447 1.1462 0.082 Uiso 1 1 calc . . .
C1 C 0.3910(6) -0.0265(9) 0.8799(15) 0.083(4) Uani 1 1 d . . .
H1A H 0.3792 0.0087 0.8017 0.124 Uiso 1 1 calc . . .
H1B H 0.3613 -0.0328 0.9477 0.124 Uiso 1 1 calc . . .
H1C H 0.4014 -0.0810 0.8435 0.124 Uiso 1 1 calc . . .


_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 I1 3.1759(10) . ?
Pb1 I1 3.1785(9) 2 ?
Pb1 I6 3.2195(11) . ?
Pb1 I7 3.2355(9) . ?
Pb1 I2 3.2585(12) . ?
Pb1 I5 3.2705(9) . ?
Pb2 I4 3.0457(13) . ?
Pb2 I3 3.0509(13) . ?
Pb2 I6 3.2768(10) . ?
Pb2 I6 3.2768(10) 7_565 ?
Pb2 I5 3.4105(13) . ?
I7 Pb1 3.2355(9) 7_565 ?
I5 Pb1 3.2705(9) 7_565 ?
I2 Pb1 3.2584(12) 7_565 ?
I1 Pb1 3.1785(9) 2_554 ?
N1 C3 1.472(14) . ?
N1 C2 1.487(13) . ?
N1 C4 1.489(12) . ?
N1 C1 1.565(15) . ?
C4 C2 1.535(16) 5_657 ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C2 C4 1.535(16) 5_657 ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 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
I1 Pb1 I1 94.69(2) . 2 ?
I1 Pb1 I6 91.56(2) . . ?
I1 Pb1 I6 98.92(3) 2 . ?
I1 Pb1 I7 86.78(3) . . ?
I1 Pb1 I7 176.37(3) 2 . ?
I6 Pb1 I7 84.33(3) . . ?
I1 Pb1 I2 100.76(3) . . ?
I1 Pb1 I2 94.15(3) 2 . ?
I6 Pb1 I2 161.24(2) . . ?
I7 Pb1 I2 82.32(3) . . ?
I1 Pb1 I5 173.42(3) . . ?
I1 Pb1 I5 91.20(3) 2 . ?
I6 Pb1 I5 84.62(2) . . ?
I7 Pb1 I5 87.51(3) . . ?
I2 Pb1 I5 81.69(3) . . ?
I4 Pb2 I3 96.84(4) . . ?
I4 Pb2 I6 97.457(17) . . ?
I3 Pb2 I6 98.513(17) . . ?
I4 Pb2 I6 97.457(17) . 7_565 ?
I3 Pb2 I6 98.512(17) . 7_565 ?
I6 Pb2 I6 155.80(3) . 7_565 ?
I4 Pb2 I5 173.80(4) . . ?
I3 Pb2 I5 89.36(4) . . ?
I6 Pb2 I5 81.559(17) . . ?
I6 Pb2 I5 81.559(17) 7_565 . ?
Pb1 I7 Pb1 79.48(3) . 7_565 ?
Pb1 I6 Pb2 81.41(2) . . ?
Pb1 I5 Pb1 78.47(3) 7_565 . ?
Pb1 I5 Pb2 78.69(3) 7_565 . ?
Pb1 I5 Pb2 78.68(3) . . ?
Pb1 I2 Pb1 78.81(4) 7_565 . ?
Pb1 I1 Pb1 169.83(4) . 2_554 ?
C3 N1 C2 115.3(9) . . ?
C3 N1 C4 114.8(9) . . ?
C2 N1 C4 105.9(9) . . ?
C3 N1 C1 107.1(10) . . ?
C2 N1 C1 107.1(9) . . ?
C4 N1 C1 106.1(8) . . ?
N1 C4 C2 109.0(9) . 5_657 ?
N1 C4 H4A 109.9 . . ?
C2 C4 H4A 109.9 5_657 . ?
N1 C4 H4B 109.9 . . ?
C2 C4 H4B 109.9 5_657 . ?
H4A C4 H4B 108.3 . . ?
N1 C3 H3A 109.5 . . ?
N1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N1 C2 C4 111.8(10) . 5_657 ?
N1 C2 H2A 109.3 . . ?
C4 C2 H2A 109.3 5_657 . ?
N1 C2 H2B 109.3 . . ?
C4 C2 H2B 109.3 5_657 . ?
H2A C2 H2B 107.9 . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.178 0.250 -0.038 143.2 29.5
2 0.822 0.750 0.038 143.3 28.7
3 0.322 0.750 0.462 143.2 28.0
4 0.678 0.250 0.538 143.3 30.1

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         2.776
_refine_diff_density_min         -1.616
_refine_diff_density_rms         0.318
####################################################################### 
# 
# 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_C8N2H19Pb3I9
_database_code_depnum_ccdc_archive 'CCDC 1902194'
loop_
_audit_author_name
_audit_author_address
'Xiao-Wu Lei'
;CCDC
China
;
_audit_update_record             
;
2019-03-10 deposited with the CCDC.	2019-08-09 downloaded from the CCDC.
;
#================================================ 

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         C8N2H19Pb3I9
_chemical_formula_sum            'C8 H19 I9 N2 Pb3'
_chemical_formula_weight         1906.92

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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   C222(1)

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

_cell_length_a                   9.2418(14)
_cell_length_b                   23.535(4)
_cell_length_c                   15.709(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3417.0(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    7006
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      25.92

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.707
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3216
_exptl_absorpt_coefficient_mu    22.876
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2326
_exptl_absorpt_correction_T_max  0.2619
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19563
_diffrn_reflns_av_R_equivalents  0.0579
_diffrn_reflns_av_sigmaI/netI    0.0504
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.37
_diffrn_reflns_theta_max         27.60
_reflns_number_total             3899
_reflns_number_gt                3471
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0411P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00042(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.012(6)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         3899
_refine_ls_number_parameters     108
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0340
_refine_ls_wR_factor_ref         0.0816
_refine_ls_wR_factor_gt          0.0794
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_restrained_S_all      0.974
_refine_ls_shift/su_max          0.002
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 1.0000 1.550405(19) 0.7500 0.03751(13) Uani 1 2 d S . .
Pb2 Pb 1.01232(5) 1.707327(15) 0.87978(2) 0.04107(12) Uani 1 1 d . . .
I5 I 0.75232(6) 1.65849(3) 0.75841(5) 0.04253(16) Uani 1 1 d . . .
I4 I 0.999(3) 1.81534(5) 0.7602(10) 0.060(2) Uani 0.50 1 d P . .
I3 I 0.76508(8) 1.46138(3) 0.76761(4) 0.0511(2) Uani 1 1 d . . .
I2 I 1.03195(8) 1.58147(4) 0.95371(5) 0.0549(2) Uani 1 1 d . . .
I1 I 0.77432(10) 1.74149(5) 1.01607(7) 0.0779(3) Uani 1 1 d . . .
N1 N 1.5015(15) 1.5514(5) 0.9856(6) 0.070(3) Uani 1 1 d . . .
C4 C 1.4334(13) 1.5233(6) 0.9118(7) 0.054(3) Uani 1 1 d . . .
H4A H 1.4909 1.5294 0.8609 0.065 Uiso 1 1 calc . . .
H4B H 1.3373 1.5386 0.9021 0.065 Uiso 1 1 calc . . .
C3 C 1.4248(14) 1.4600(6) 0.9324(8) 0.057(3) Uani 1 1 d . . .
H3A H 1.3243 1.4485 0.9371 0.069 Uiso 1 1 calc . . .
H3B H 1.4691 1.4382 0.8870 0.069 Uiso 1 1 calc . . .
C2 C 1.499(3) 1.6172(7) 0.9681(14) 0.157(11) Uani 1 1 d . . .
H2A H 1.5538 1.6253 0.9175 0.235 Uiso 1 1 calc R . .
H2B H 1.5415 1.6369 1.0155 0.235 Uiso 1 1 calc R . .
H2C H 1.4012 1.6296 0.9605 0.235 Uiso 1 1 calc R . .
C1 C 1.6520(14) 1.5329(12) 0.9931(14) 0.18(2) Uani 1 1 d . . .
H1A H 1.6981 1.5517 1.0409 0.220 Uiso 1 1 calc R . .
H1B H 1.7050 1.5424 0.9417 0.220 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
Pb1 I3 3.0300(8) . ?
Pb1 I3 3.0300(8) 3_756 ?
Pb1 I2 3.2959(9) . ?
Pb1 I2 3.2959(10) 3_756 ?
Pb1 I5 3.4246(8) 3_756 ?
Pb1 I5 3.4246(8) . ?
Pb2 I1 3.1609(10) 8_587 ?
Pb2 I4 3.164(10) . ?
Pb2 I1 3.1730(10) . ?
Pb2 I2 3.1868(10) . ?
Pb2 I5 3.2758(9) . ?
Pb2 I5 3.2811(8) 3_756 ?
Pb2 I4 3.363(10) 3_756 ?
I5 Pb2 3.2811(8) 3_756 ?
I4 I4 0.32(3) 3_756 ?
I4 Pb2 3.363(10) 3_756 ?
I1 Pb2 3.1609(9) 8_487 ?
N1 C1 1.46(2) . ?
N1 C4 1.476(17) . ?
N1 C3 1.495(14) 4_587 ?
N1 C2 1.573(19) . ?
C4 C3 1.527(19) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C3 N1 1.495(14) 4_587 ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C1 C1 1.56(6) 4_587 ?
C1 H1A 0.9700 . ?
C1 H1B 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
I3 Pb1 I3 92.49(3) . 3_756 ?
I3 Pb1 I2 97.408(19) . . ?
I3 Pb1 I2 100.25(2) 3_756 . ?
I3 Pb1 I2 100.25(2) . 3_756 ?
I3 Pb1 I2 97.406(19) 3_756 3_756 ?
I2 Pb1 I2 154.37(3) . 3_756 ?
I3 Pb1 I5 174.96(2) . 3_756 ?
I3 Pb1 I5 91.79(2) 3_756 3_756 ?
I2 Pb1 I5 79.21(2) . 3_756 ?
I2 Pb1 I5 81.82(2) 3_756 3_756 ?
I3 Pb1 I5 91.79(2) . . ?
I3 Pb1 I5 174.96(2) 3_756 . ?
I2 Pb1 I5 81.82(2) . . ?
I2 Pb1 I5 79.21(2) 3_756 . ?
I5 Pb1 I5 84.06(3) 3_756 . ?
I1 Pb2 I4 91.8(4) 8_587 . ?
I1 Pb2 I1 94.887(15) 8_587 . ?
I4 Pb2 I1 99.8(4) . . ?
I1 Pb2 I2 97.01(3) 8_587 . ?
I4 Pb2 I2 164.9(2) . . ?
I1 Pb2 I2 91.67(3) . . ?
I1 Pb2 I5 175.51(3) 8_587 . ?
I4 Pb2 I5 84.7(4) . . ?
I1 Pb2 I5 88.46(3) . . ?
I2 Pb2 I5 85.86(2) . . ?
I1 Pb2 I5 88.18(3) 8_587 3_756 ?
I4 Pb2 I5 85.1(4) . 3_756 ?
I1 Pb2 I5 174.13(3) . 3_756 ?
I2 Pb2 I5 82.98(2) . 3_756 ?
I5 Pb2 I5 88.75(2) . 3_756 ?
I1 Pb2 I4 94.2(4) 8_587 3_756 ?
I4 Pb2 I4 4.4(4) . 3_756 ?
I1 Pb2 I4 103.2(4) . 3_756 ?
I2 Pb2 I4 160.5(2) . 3_756 ?
I5 Pb2 I4 82.1(4) . 3_756 ?
I5 Pb2 I4 81.5(3) 3_756 3_756 ?
Pb2 I5 Pb2 77.05(2) . 3_756 ?
Pb2 I5 Pb1 78.041(18) . . ?
Pb2 I5 Pb1 77.971(17) 3_756 . ?
I4 I4 Pb2 126.1(12) 3_756 . ?
I4 I4 Pb2 49.5(12) 3_756 3_756 ?
Pb2 I4 Pb2 77.41(4) . 3_756 ?
Pb2 I2 Pb1 81.21(2) . . ?
Pb2 I1 Pb2 167.65(4) 8_487 . ?
C1 N1 C4 109.6(13) . . ?
C1 N1 C3 109.2(13) . 4_587 ?
C4 N1 C3 113.2(10) . 4_587 ?
C1 N1 C2 108.7(17) . . ?
C4 N1 C2 107.4(13) . . ?
C3 N1 C2 108.7(12) 4_587 . ?
N1 C4 C3 107.0(9) . . ?
N1 C4 H4A 110.3 . . ?
C3 C4 H4A 110.3 . . ?
N1 C4 H4B 110.3 . . ?
C3 C4 H4B 110.3 . . ?
H4A C4 H4B 108.6 . . ?
N1 C3 C4 109.5(10) 4_587 . ?
N1 C3 H3A 109.8 4_587 . ?
C4 C3 H3A 109.8 . . ?
N1 C3 H3B 109.8 4_587 . ?
C4 C3 H3B 109.8 . . ?
H3A C3 H3B 108.2 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N1 C1 C1 107.8(11) . 4_587 ?
N1 C1 H1A 110.1 . . ?
C1 C1 H1A 110.1 4_587 . ?
N1 C1 H1B 110.1 . . ?
C1 C1 H1B 110.1 4_587 . ?
H1A C1 H1B 108.5 . . ?

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.000 0.680 0.250 118.3 44.5
2 0.000 0.320 0.750 118.3 41.8
3 0.500 0.180 0.250 118.3 44.5
4 0.500 0.820 0.750 118.3 41.8

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        27.60
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         1.785
_refine_diff_density_min         -4.362
_refine_diff_density_rms         0.219
