# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2022

####################################################################### 
# 
# 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_r-3
_database_code_depnum_ccdc_archive 'CCDC 2169490'
loop_
_audit_author_name
_audit_author_address
'Congcong Chen'
;Southern University of Science and Technology
China
;
_audit_update_record             
;
2022-04-29 deposited with the CCDC.	2022-08-05 downloaded from the CCDC.
;
_audit_creation_date             2022-02-16
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'I2 Pb0.5, I Pb0.167, 0.333(I), C3 H11 N3 S'
_chemical_formula_sum            'C3 H11 I3.33 N3 Pb0.67 S'
_chemical_formula_weight         682.33
_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'
I I -0.4742 1.8119 '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'
S S 0.1246 0.1234 '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      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3'
_space_group_name_Hall           '-R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   15.0135(19)
_cell_length_b                   15.0135(19)
_cell_length_c                   31.781(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     6203.8(18)
_cell_formula_units_Z            18
_cell_measurement_reflns_used    2096
_cell_measurement_temperature    299.11
_cell_measurement_theta_max      29.62
_cell_measurement_theta_min      2.71
_shelx_estimated_absorpt_T_max   0.365
_shelx_estimated_absorpt_T_min   0.294
_exptl_absorpt_coefficient_mu    15.764
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.2981
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.287
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             5352
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.103
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_unetI/netI     0.0672
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            5926
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.493
_diffrn_reflns_theta_min         1.692
_diffrn_ambient_temperature      299.11
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_voltage           40.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3054
_reflns_number_total             4081
_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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_refine_diff_density_max         1.842
_refine_diff_density_min         -3.754
_refine_diff_density_rms         0.452
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     102
_refine_ls_number_reflns         4081
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0398
_refine_ls_restrained_S_all      0.985
_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)+(0.0352P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0920
_refine_ls_wR_factor_ref         0.0997
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups, All N(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1D,H1E), C2(H2C,H2D)
2.b X=CH2 refined with riding coordinates:
 N2(H2A,H2B), N3(H3A,H3B)
2.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_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
Pb1 Pb 0.333333 0.666667 0.29932(2) 0.02758(11) Uani 1 3 d S T P . .
Pb2 Pb 0.333333 0.666667 0.166667 0.03722(17) Uani 1 6 d S T P . .
I1 I 0.52659(3) 0.69546(4) 0.35520(2) 0.03353(12) Uani 1 1 d . . . . .
I2 I 0.34821(4) 0.51106(4) 0.23542(2) 0.04494(15) Uani 1 1 d . . . . .
Pb3 Pb 0.666667 0.333333 0.333333 0.02829(14) Uani 1 6 d S T P . .
I3 I 0.49436(4) 0.33963(4) 0.27596(2) 0.04055(13) Uani 1 1 d . . . . .
I4 I 0.666667 0.333333 0.53684(3) 0.0502(2) Uani 1 3 d S T P . .
S1 S 0.2905(2) 0.3212(3) 0.47402(8) 0.0677(8) Uani 1 1 d . . . . .
N1 N 0.3826(5) 0.4231(5) 0.3546(2) 0.0408(15) Uani 1 1 d . . . . .
H1A H 0.319999 0.400441 0.344031 0.049 Uiso 1 1 calc R U . . .
H1B H 0.405796 0.381526 0.346583 0.049 Uiso 1 1 calc R U . . .
H1C H 0.424827 0.486382 0.345120 0.049 Uiso 1 1 calc R U . . .
N2 N 0.4677(8) 0.3167(8) 0.4720(3) 0.088(3) Uani 1 1 d . . . . .
H2A H 0.520473 0.319157 0.483795 0.106 Uiso 1 1 calc R U . . .
H2B H 0.457101 0.304150 0.445551 0.106 Uiso 1 1 calc R U . . .
N3 N 0.4208(6) 0.3510(7) 0.5342(2) 0.063(2) Uani 1 1 d . . . . .
H3A H 0.473452 0.353452 0.546097 0.076 Uiso 1 1 calc R U . . .
H3B H 0.378442 0.361071 0.548880 0.076 Uiso 1 1 calc R U . . .
C1 C 0.3780(6) 0.4247(6) 0.4018(3) 0.0456(19) Uani 1 1 d . . . . .
H1D H 0.445831 0.448028 0.413498 0.055 Uiso 1 1 calc R U . . .
H1E H 0.355285 0.471931 0.410732 0.055 Uiso 1 1 calc R U . . .
C2 C 0.3049(6) 0.3191(7) 0.4172(2) 0.051(2) Uani 1 1 d . . . . .
H2C H 0.330411 0.273091 0.410070 0.061 Uiso 1 1 calc R U . . .
H2D H 0.238537 0.293831 0.403751 0.061 Uiso 1 1 calc R U . . .
C3 C 0.4050(7) 0.3318(6) 0.4940(3) 0.0443(19) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 I1 3.2412(6) 2_665 ?
Pb1 I1 3.2412(6) 3_565 ?
Pb1 I1 3.2412(6) . ?
Pb1 I2 3.1865(6) 3_565 ?
Pb1 I2 3.1865(6) 2_665 ?
Pb1 I2 3.1865(6) . ?
Pb2 I2 3.2869(6) 13_565 ?
Pb2 I2 3.2868(6) 14_455 ?
Pb2 I2 3.2869(6) 2_665 ?
Pb2 I2 3.2868(6) 15 ?
Pb2 I2 3.2869(6) 3_565 ?
Pb2 I2 3.2869(6) . ?
Pb3 I3 3.2047(6) 2_655 ?
Pb3 I3 3.2046(6) 17 ?
Pb3 I3 3.2047(6) 18_545 ?
Pb3 I3 3.2047(6) 3_665 ?
Pb3 I3 3.2047(6) 16_655 ?
Pb3 I3 3.2048(6) . ?
S1 C2 1.820(8) . ?
S1 C3 1.763(9) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C1 1.504(11) . ?
N2 H2A 0.8600 . ?
N2 H2B 0.8600 . ?
N2 C3 1.279(11) . ?
N3 H3A 0.8600 . ?
N3 H3B 0.8600 . ?
N3 C3 1.308(11) . ?
C1 H1D 0.9700 . ?
C1 H1E 0.9700 . ?
C1 C2 1.490(11) . ?
C2 H2C 0.9700 . ?
C2 H2D 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
I1 Pb1 I1 92.842(16) 2_665 3_565 ?
I1 Pb1 I1 92.842(16) 2_665 . ?
I1 Pb1 I1 92.843(16) 3_565 . ?
I2 Pb1 I1 89.670(15) 3_565 2_665 ?
I2 Pb1 I1 173.070(17) 2_665 3_565 ?
I2 Pb1 I1 89.669(15) 2_665 . ?
I2 Pb1 I1 93.483(15) 2_665 2_665 ?
I2 Pb1 I1 173.069(18) 3_565 . ?
I2 Pb1 I1 173.070(17) . 2_665 ?
I2 Pb1 I1 93.483(16) . . ?
I2 Pb1 I1 93.483(15) 3_565 3_565 ?
I2 Pb1 I1 89.669(15) . 3_565 ?
I2 Pb1 I2 83.728(19) 3_565 . ?
I2 Pb1 I2 83.729(19) 3_565 2_665 ?
I2 Pb1 I2 83.729(19) 2_665 . ?
I2 Pb2 I2 80.631(15) 13_565 15 ?
I2 Pb2 I2 80.631(16) 13_565 14_455 ?
I2 Pb2 I2 80.632(16) 14_455 15 ?
I2 Pb2 I2 80.629(16) 3_565 . ?
I2 Pb2 I2 99.370(16) 2_665 15 ?
I2 Pb2 I2 80.630(16) 2_665 . ?
I2 Pb2 I2 99.370(16) . 14_455 ?
I2 Pb2 I2 99.369(16) 3_565 13_565 ?
I2 Pb2 I2 180.0 3_565 15 ?
I2 Pb2 I2 99.369(16) 2_665 13_565 ?
I2 Pb2 I2 99.371(16) . 15 ?
I2 Pb2 I2 180.0 . 13_565 ?
I2 Pb2 I2 99.369(16) 3_565 14_455 ?
I2 Pb2 I2 80.630(16) 3_565 2_665 ?
I2 Pb2 I2 180.0 2_665 14_455 ?
Pb1 I2 Pb2 81.253(16) . . ?
I3 Pb3 I3 90.827(15) 16_655 17 ?
I3 Pb3 I3 180.0 16_655 . ?
I3 Pb3 I3 90.825(15) 2_655 3_665 ?
I3 Pb3 I3 90.825(15) 2_655 . ?
I3 Pb3 I3 89.173(15) 2_655 16_655 ?
I3 Pb3 I3 89.175(15) 17 . ?
I3 Pb3 I3 89.174(15) 3_665 16_655 ?
I3 Pb3 I3 90.828(15) 18_545 17 ?
I3 Pb3 I3 89.173(15) 2_655 18_545 ?
I3 Pb3 I3 90.825(15) 3_665 . ?
I3 Pb3 I3 180.0 3_665 18_545 ?
I3 Pb3 I3 89.175(15) 18_545 . ?
I3 Pb3 I3 180.0 2_655 17 ?
I3 Pb3 I3 89.174(15) 3_665 17 ?
I3 Pb3 I3 90.826(15) 16_655 18_545 ?
C3 S1 C2 103.9(4) . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
H2A N2 H2B 120.0 . . ?
C3 N2 H2A 120.0 . . ?
C3 N2 H2B 120.0 . . ?
H3A N3 H3B 120.0 . . ?
C3 N3 H3A 120.0 . . ?
C3 N3 H3B 120.0 . . ?
N1 C1 H1D 109.9 . . ?
N1 C1 H1E 109.9 . . ?
H1D C1 H1E 108.3 . . ?
C2 C1 N1 109.1(7) . . ?
C2 C1 H1D 109.9 . . ?
C2 C1 H1E 109.9 . . ?
S1 C2 H2C 109.7 . . ?
S1 C2 H2D 109.7 . . ?
C1 C2 S1 109.8(6) . . ?
C1 C2 H2C 109.7 . . ?
C1 C2 H2D 109.7 . . ?
H2C C2 H2D 108.2 . . ?
N2 C3 S1 124.0(7) . . ?
N2 C3 N3 120.2(9) . . ?
N3 C3 S1 115.7(7) . . ?

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 S1 -175.6(6) . . . . ?
C2 S1 C3 N2 -14.0(10) . . . . ?
C2 S1 C3 N3 169.8(7) . . . . ?
C3 S1 C2 C1 -75.7(7) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_a
_database_code_depnum_ccdc_archive 'CCDC 2169491'
loop_
_audit_author_name
_audit_author_address
'Congcong Chen'
;Southern University of Science and Technology
China
;
_audit_update_record             
;
2022-04-29 deposited with the CCDC.	2022-08-05 downloaded from the CCDC.
;
_audit_creation_date             2022-02-21
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Ge I6, 2(Ge I3), 2(I), Ge2 I4, 4(C3 H11 N3 S)'
_chemical_formula_sum            'C12 H44 Ge5 I18 N12 S4'
_chemical_formula_weight         3131.98
_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'
Ge Ge 0.1547 1.8001 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.6160(5)
_cell_length_b                   10.9195(6)
_cell_length_c                   18.0200(11)
_cell_angle_alpha                81.199(2)
_cell_angle_beta                 87.561(2)
_cell_angle_gamma                70.561(2)
_cell_volume                     1579.84(16)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    9891
_cell_measurement_temperature    298.0
_cell_measurement_theta_max      25.389
_cell_measurement_theta_min      2.446
_shelx_estimated_absorpt_T_max   0.480
_shelx_estimated_absorpt_T_min   0.317
_exptl_absorpt_coefficient_mu    11.303
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.3568
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1438 before and 0.0719 after correction.
The Ratio of minimum to maximum transmission is 0.4788.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.292
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1378
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.132
_exptl_crystal_size_mid          0.085
_exptl_crystal_size_min          0.076
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0525
_diffrn_reflns_av_unetI/netI     0.0462
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19386
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.407
_diffrn_reflns_theta_min         2.446
_diffrn_ambient_temperature      298.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5116
_reflns_number_total             5808
_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       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.320
_refine_diff_density_min         -4.847
_refine_diff_density_rms         0.688
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.232
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     234
_refine_ls_number_reflns         5808
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0466
_refine_ls_restrained_S_all      1.234
_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)+(0.0628P)²+0.5676P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1144
_refine_ls_wR_factor_ref         0.1190
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups, All N(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C2(H2C,H2D), C3(H3D,H3E), C5(H5C,H5D), C6(H6D,H6E)
3.b X=CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B), N4(H4A,H4B), N5(H5A,H5B)
3.c Idealised Me refined as rotating group:
 N3(H3A,H3B,H3C), N6(H6A,H6B,H6C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
I1 I 0.72524(6) 0.58366(5) 0.38527(3) 0.03280(15) Uani 1 1 d . . . . .
I2 I 0.79265(6) 0.36359(5) 0.59503(3) 0.03087(15) Uani 1 1 d . . . . .
I3 I 0.84061(6) 0.74377(4) 0.56776(3) 0.02780(14) Uani 1 1 d . . . . .
I4 I 0.64951(7) 1.04328(5) 0.68279(3) 0.03297(15) Uani 1 1 d . . . . .
I5 I 0.85100(6) 1.20940(5) 0.83454(3) 0.03480(16) Uani 1 1 d . . . . .
I6 I 0.34573(6) 1.22728(5) 0.84129(3) 0.03342(15) Uani 1 1 d . . . . .
I7 I 0.48378(7) 0.59154(5) 0.77317(3) 0.03737(16) Uani 1 1 d . . . . .
I8 I 0.35068(7) 0.85590(5) 0.95745(3) 0.03729(16) Uani 1 1 d . . . . .
I9 I 0.25653(6) 0.49860(5) 1.01268(3) 0.03789(16) Uani 1 1 d . . . . .
Ge1 Ge 1.000000 0.500000 0.500000 0.0257(3) Uani 1 2 d S . P . .
Ge2 Ge 0.57051(10) 1.28687(8) 0.72809(5) 0.0293(2) Uani 1 1 d . . . . .
Ge3 Ge 0.43911(11) 0.64028(8) 1.07085(5) 0.0359(2) Uani 1 1 d . . . . .
S1 S 0.1306(3) 0.8864(2) 0.64346(14) 0.0409(5) Uani 1 1 d . . . . .
S2 S 0.0248(3) 0.7707(2) 0.84755(14) 0.0460(6) Uani 1 1 d . . . . .
N1 N 0.2112(11) 1.1018(7) 0.6420(6) 0.068(3) Uani 1 1 d . . . . .
H1A H 0.247145 1.154229 0.661726 0.082 Uiso 1 1 calc R U . . .
H1B H 0.173986 1.122966 0.596624 0.082 Uiso 1 1 calc R U . . .
N2 N 0.2679(11) 0.9556(8) 0.7486(5) 0.055(2) Uani 1 1 d . . . . .
H2A H 0.304572 1.006201 0.769677 0.066 Uiso 1 1 calc R U . . .
H2B H 0.267853 0.881491 0.772915 0.066 Uiso 1 1 calc R U . . .
N3 N 0.4446(8) 0.6895(7) 0.5679(4) 0.0409(18) Uani 1 1 d . . . . .
H3A H 0.392849 0.650008 0.542901 0.049 Uiso 1 1 calc R U . . .
H3B H 0.424166 0.675306 0.616741 0.049 Uiso 1 1 calc R U . . .
H3C H 0.552452 0.657151 0.560394 0.049 Uiso 1 1 calc R U . . .
N4 N -0.0834(11) 0.8453(11) 0.9741(5) 0.075(3) Uani 1 1 d . . . . .
H4A H -0.153759 0.886952 1.004532 0.090 Uiso 1 1 calc R U . . .
H4B H 0.016684 0.803891 0.988608 0.090 Uiso 1 1 calc R U . . .
N5 N -0.2777(10) 0.9064(10) 0.8844(6) 0.068(3) Uani 1 1 d . . . . .
H5A H -0.348885 0.948404 0.914392 0.082 Uiso 1 1 calc R U . . .
H5B H -0.306261 0.905578 0.839356 0.082 Uiso 1 1 calc R U . . .
N6 N -0.0752(10) 0.5027(7) 0.7444(5) 0.0462(19) Uani 1 1 d . . . . .
H6A H -0.092431 0.553324 0.699830 0.055 Uiso 1 1 calc R U . . .
H6B H -0.169977 0.494903 0.762071 0.055 Uiso 1 1 calc R U . . .
H6C H -0.004440 0.423718 0.739563 0.055 Uiso 1 1 calc R U . . .
C1 C 0.2132(10) 0.9909(8) 0.6806(6) 0.039(2) Uani 1 1 d . . . . .
C2 C 0.2036(10) 0.8927(8) 0.5484(5) 0.039(2) Uani 1 1 d . . . . .
H2C H 0.149217 0.848698 0.520771 0.047 Uiso 1 1 calc R U . . .
H2D H 0.171797 0.983813 0.525249 0.047 Uiso 1 1 calc R U . . .
C3 C 0.3857(11) 0.8314(8) 0.5411(5) 0.040(2) Uani 1 1 d . . . . .
H3D H 0.415179 0.846345 0.488715 0.048 Uiso 1 1 calc R U . . .
H3E H 0.440744 0.873910 0.569364 0.048 Uiso 1 1 calc R U . . .
C4 C -0.1279(11) 0.8448(8) 0.9069(5) 0.039(2) Uani 1 1 d . . . . .
C5 C -0.0859(15) 0.7029(10) 0.7918(6) 0.067(3) Uani 1 1 d . U . . .
H5C H -0.198144 0.721554 0.809457 0.081 Uiso 1 1 calc R U . . .
H5D H -0.089319 0.743341 0.739813 0.081 Uiso 1 1 calc R U . . .
C6 C -0.0067(14) 0.5628(9) 0.7970(6) 0.053(3) Uani 1 1 d . . . . .
H6D H -0.017382 0.522218 0.847850 0.064 Uiso 1 1 calc R U . . .
H6E H 0.109764 0.544728 0.787079 0.064 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
I1 Ge1 3.0186(5) . ?
I2 Ge1 3.0121(5) . ?
I3 Ge1 2.9801(5) . ?
I4 Ge2 2.7598(9) . ?
I5 Ge2 2.9619(10) . ?
I6 Ge2 2.9037(10) . ?
I8 Ge3 2.7868(10) . ?
I9 Ge3 2.8676(11) . ?
I9 Ge3 3.0261(11) 2_667 ?
S1 C1 1.752(8) . ?
S1 C2 1.798(9) . ?
S2 C4 1.722(9) . ?
S2 C5 1.802(10) . ?
N1 H1A 0.8600 . ?
N1 H1B 0.8600 . ?
N1 C1 1.296(11) . ?
N2 H2A 0.8600 . ?
N2 H2B 0.8600 . ?
N2 C1 1.287(12) . ?
N3 H3A 0.8900 . ?
N3 H3B 0.8900 . ?
N3 H3C 0.8900 . ?
N3 C3 1.470(10) . ?
N4 H4A 0.8600 . ?
N4 H4B 0.8600 . ?
N4 C4 1.288(13) . ?
N5 H5A 0.8600 . ?
N5 H5B 0.8600 . ?
N5 C4 1.291(12) . ?
N6 H6A 0.8900 . ?
N6 H6B 0.8900 . ?
N6 H6C 0.8900 . ?
N6 C6 1.474(12) . ?
C2 H2C 0.9700 . ?
C2 H2D 0.9700 . ?
C2 C3 1.496(11) . ?
C3 H3D 0.9700 . ?
C3 H3E 0.9700 . ?
C5 H5C 0.9700 . ?
C5 H5D 0.9700 . ?
C5 C6 1.442(13) . ?
C6 H6D 0.9700 . ?
C6 H6E 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
Ge3 I9 Ge3 88.85(3) . 2_667 ?
I1 Ge1 I1 180.0 2_766 . ?
I2 Ge1 I1 85.876(15) . . ?
I2 Ge1 I1 85.877(15) 2_766 2_766 ?
I2 Ge1 I1 94.124(15) 2_766 . ?
I2 Ge1 I1 94.123(15) . 2_766 ?
I2 Ge1 I2 180.000(17) . 2_766 ?
I3 Ge1 I1 89.811(15) 2_766 . ?
I3 Ge1 I1 89.810(15) . 2_766 ?
I3 Ge1 I1 90.190(15) . . ?
I3 Ge1 I1 90.189(15) 2_766 2_766 ?
I3 Ge1 I2 89.385(14) 2_766 . ?
I3 Ge1 I2 90.615(14) 2_766 2_766 ?
I3 Ge1 I2 89.385(14) . 2_766 ?
I3 Ge1 I2 90.615(14) . . ?
I3 Ge1 I3 180.0 2_766 . ?
I4 Ge2 I5 94.95(3) . . ?
I4 Ge2 I6 92.21(3) . . ?
I6 Ge2 I5 93.99(3) . . ?
I8 Ge3 I9 92.04(3) . 2_667 ?
I8 Ge3 I9 96.22(3) . . ?
I9 Ge3 I9 91.15(3) . 2_667 ?
C1 S1 C2 102.7(4) . . ?
C4 S2 C5 100.8(6) . . ?
H1A N1 H1B 120.0 . . ?
C1 N1 H1A 120.0 . . ?
C1 N1 H1B 120.0 . . ?
H2A N2 H2B 120.0 . . ?
C1 N2 H2A 120.0 . . ?
C1 N2 H2B 120.0 . . ?
H3A N3 H3B 109.5 . . ?
H3A N3 H3C 109.5 . . ?
H3B N3 H3C 109.5 . . ?
C3 N3 H3A 109.5 . . ?
C3 N3 H3B 109.5 . . ?
C3 N3 H3C 109.5 . . ?
H4A N4 H4B 120.0 . . ?
C4 N4 H4A 120.0 . . ?
C4 N4 H4B 120.0 . . ?
H5A N5 H5B 120.0 . . ?
C4 N5 H5A 120.0 . . ?
C4 N5 H5B 120.0 . . ?
H6A N6 H6B 109.5 . . ?
H6A N6 H6C 109.5 . . ?
H6B N6 H6C 109.5 . . ?
C6 N6 H6A 109.5 . . ?
C6 N6 H6B 109.5 . . ?
C6 N6 H6C 109.5 . . ?
N1 C1 S1 120.9(8) . . ?
N2 C1 S1 117.1(7) . . ?
N2 C1 N1 121.9(9) . . ?
S1 C2 H2C 108.6 . . ?
S1 C2 H2D 108.6 . . ?
H2C C2 H2D 107.6 . . ?
C3 C2 S1 114.6(6) . . ?
C3 C2 H2C 108.6 . . ?
C3 C2 H2D 108.6 . . ?
N3 C3 C2 113.0(7) . . ?
N3 C3 H3D 109.0 . . ?
N3 C3 H3E 109.0 . . ?
C2 C3 H3D 109.0 . . ?
C2 C3 H3E 109.0 . . ?
H3D C3 H3E 107.8 . . ?
N4 C4 S2 116.7(7) . . ?
N4 C4 N5 120.7(10) . . ?
N5 C4 S2 122.4(8) . . ?
S2 C5 H5C 109.6 . . ?
S2 C5 H5D 109.6 . . ?
H5C C5 H5D 108.1 . . ?
C6 C5 S2 110.2(7) . . ?
C6 C5 H5C 109.6 . . ?
C6 C5 H5D 109.6 . . ?
N6 C6 H6D 108.9 . . ?
N6 C6 H6E 108.9 . . ?
C5 C6 N6 113.5(8) . . ?
C5 C6 H6D 108.9 . . ?
C5 C6 H6E 108.9 . . ?
H6D C6 H6E 107.7 . . ?

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
S1 C2 C3 N3 64.0(9) . . . . ?
S2 C5 C6 N6 -171.5(8) . . . . ?
C1 S1 C2 C3 67.5(7) . . . . ?
C2 S1 C1 N1 42.6(9) . . . . ?
C2 S1 C1 N2 -140.7(8) . . . . ?
C4 S2 C5 C6 -122.6(9) . . . . ?
C5 S2 C4 N4 146.1(8) . . . . ?
C5 S2 C4 N5 -39.3(9) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_a_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2169492'
loop_
_audit_author_name
_audit_author_address
'Congcong Chen'
;Southern University of Science and Technology
China
;
_audit_update_record             
;
2022-04-29 deposited with the CCDC.	2022-08-05 downloaded from the CCDC.
;
_audit_creation_date             2022-02-21
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(Ge I3), 2(I), 2(C3 H11 N3 S)'
_chemical_formula_sum            'C6 H22 Ge2 I8 N6 S2'
_chemical_formula_weight         1402.79
_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'
Ge Ge 0.1547 1.8001 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   19.178(3)
_cell_length_b                   12.2635(17)
_cell_length_c                   25.280(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5945.7(15)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9193
_cell_measurement_temperature    298.0
_cell_measurement_theta_max      25.373
_cell_measurement_theta_min      2.546
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    10.477
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.3700
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1488 before and 0.0627 after correction.
The Ratio of minimum to maximum transmission is 0.4965.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    3.134
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4960
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.91
_exptl_crystal_size_mid          0.103
_exptl_crystal_size_min          0.086
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0514
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            41787
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.419
_diffrn_reflns_theta_min         2.124
_diffrn_ambient_temperature      298.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4503
_reflns_number_total             5466
_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       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         2.086
_refine_diff_density_min         -3.614
_refine_diff_density_rms         0.843
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.204
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         5466
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0366
_refine_ls_restrained_S_all      1.208
_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)+(0.0516P)²+6.3482P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0869
_refine_ls_wR_factor_ref         0.0999
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups, All N(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N2) \\sim Ueq, Uanis(N1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C2(H2C,H2D), C3(H3D,H3E), C5(H5C,H5D), C6(H6D,H6E)
3.b X=CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B), N4(H4A,H4B), N5(H5A,H5B)
3.c Idealised Me refined as rotating group:
 N3(H3A,H3B,H3C), N6(H6A,H6B,H6C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
I1 I 0.37282(3) -0.01903(4) 0.52133(2) 0.04014(15) Uani 1 1 d . . . . .
I2 I 0.16262(3) -0.04781(4) 0.50519(2) 0.03747(15) Uani 1 1 d . . . . .
I3 I 0.24027(3) 0.19144(4) 0.60173(2) 0.03893(15) Uani 1 1 d . . . . .
I4 I 0.58623(3) 0.00696(4) 0.65366(2) 0.03952(15) Uani 1 1 d . . . . .
I6 I 0.52093(3) 0.68958(4) 0.73013(2) 0.04031(15) Uani 1 1 d . . . . .
I7 I 0.63571(3) 0.44118(4) 0.80676(2) 0.04509(16) Uani 1 1 d . . . . .
I8 I 0.59132(3) 0.41663(6) 0.65076(2) 0.0600(2) Uani 1 1 d . . . . .
Ge1 Ge 0.25128(4) -0.03309(6) 0.59102(3) 0.03020(19) Uani 1 1 d . . . . .
Ge2 Ge 0.51286(4) 0.46153(6) 0.74056(3) 0.03008(19) Uani 1 1 d . . . . .
S1 S 0.53799(12) 0.32108(18) 0.50782(9) 0.0455(5) Uani 1 1 d . . . . .
S2 S 0.77149(15) 0.19002(18) 0.63354(10) 0.0579(6) Uani 1 1 d . . . . .
N1 N 0.4701(5) 0.2076(7) 0.4340(4) 0.095(3) Uani 1 1 d . U . . .
H1A H 0.458573 0.194039 0.401808 0.114 Uiso 1 1 calc R U . . .
H1B H 0.454554 0.167293 0.459203 0.114 Uiso 1 1 calc R U . . .
N2 N 0.5353(5) 0.3510(11) 0.4089(4) 0.120(4) Uani 1 1 d . U . . .
H2A H 0.524569 0.339045 0.376411 0.145 Uiso 1 1 calc R U . . .
H2B H 0.562372 0.404438 0.416946 0.145 Uiso 1 1 calc R U . . .
N3 N 0.4323(3) 0.1739(6) 0.6254(3) 0.0434(16) Uani 1 1 d . . . . .
H3A H 0.423519 0.107084 0.613339 0.052 Uiso 1 1 calc R U . . .
H3B H 0.395403 0.198526 0.643046 0.052 Uiso 1 1 calc R U . . .
H3C H 0.469064 0.171826 0.646880 0.052 Uiso 1 1 calc R U . . .
N4 N 0.7102(4) 0.2520(7) 0.5466(3) 0.064(2) Uani 1 1 d . . . . .
H4A H 0.699495 0.296558 0.521629 0.077 Uiso 1 1 calc R U . . .
H4B H 0.696263 0.185447 0.545305 0.077 Uiso 1 1 calc R U . . .
N5 N 0.7687(4) 0.3844(6) 0.5886(3) 0.054(2) Uani 1 1 d . . . . .
H5A H 0.758018 0.429073 0.563714 0.064 Uiso 1 1 calc R U . . .
H5B H 0.793417 0.406212 0.614975 0.064 Uiso 1 1 calc R U . . .
N6 N 0.6811(3) 0.1827(5) 0.7437(3) 0.0474(17) Uani 1 1 d . . . . .
H6A H 0.665218 0.159017 0.712664 0.057 Uiso 1 1 calc R U . . .
H6B H 0.659866 0.244967 0.752037 0.057 Uiso 1 1 calc R U . . .
H6C H 0.672306 0.133101 0.768505 0.057 Uiso 1 1 calc R U . . .
C1 C 0.5116(4) 0.2902(8) 0.4447(4) 0.049(2) Uani 1 1 d . . . . .
C2 C 0.5062(6) 0.2120(7) 0.5505(4) 0.062(3) Uani 1 1 d . . . . .
H2C H 0.493288 0.149543 0.529092 0.075 Uiso 1 1 calc R U . . .
H2D H 0.543031 0.189515 0.574446 0.075 Uiso 1 1 calc R U . . .
C3 C 0.4473(5) 0.2472(7) 0.5804(4) 0.056(2) Uani 1 1 d . . . . .
H3D H 0.406788 0.250200 0.557449 0.067 Uiso 1 1 calc R U . . .
H3E H 0.455825 0.320197 0.593671 0.067 Uiso 1 1 calc R U . . .
C4 C 0.7478(4) 0.2855(7) 0.5866(3) 0.0345(17) Uani 1 1 d . . . . .
C5 C 0.7765(4) 0.2703(7) 0.6938(3) 0.046(2) Uani 1 1 d . . . . .
H5C H 0.823513 0.297749 0.698446 0.055 Uiso 1 1 calc R U . . .
H5D H 0.745135 0.332195 0.691375 0.055 Uiso 1 1 calc R U . . .
C6 C 0.7568(4) 0.2011(8) 0.7402(4) 0.051(2) Uani 1 1 d . . . . .
H6D H 0.780245 0.131296 0.737388 0.061 Uiso 1 1 calc R U . . .
H6E H 0.772659 0.236174 0.772384 0.061 Uiso 1 1 calc R U . . .
I5 I 0.36681(3) 0.44334(4) 0.67900(2) 0.03706(14) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I1 Ge1 2.9269(10) . ?
I2 Ge1 2.7623(10) . ?
I3 Ge1 2.7749(10) . ?
I6 Ge2 2.8133(10) . ?
I7 Ge2 2.9006(9) . ?
I8 Ge2 2.7787(10) . ?
S1 C1 1.715(9) . ?
S1 C2 1.825(9) . ?
S2 C4 1.729(8) . ?
S2 C5 1.817(9) . ?
N1 H1A 0.8600 . ?
N1 H1B 0.8600 . ?
N1 C1 1.316(12) . ?
N2 H2A 0.8600 . ?
N2 H2B 0.8600 . ?
N2 C1 1.258(12) . ?
N3 H3A 0.8900 . ?
N3 H3B 0.8900 . ?
N3 H3C 0.8900 . ?
N3 C3 1.478(10) . ?
N4 H4A 0.8600 . ?
N4 H4B 0.8600 . ?
N4 C4 1.307(10) . ?
N5 H5A 0.8600 . ?
N5 H5B 0.8600 . ?
N5 C4 1.278(10) . ?
N6 H6A 0.8900 . ?
N6 H6B 0.8900 . ?
N6 H6C 0.8900 . ?
N6 C6 1.472(10) . ?
C2 H2C 0.9700 . ?
C2 H2D 0.9700 . ?
C2 C3 1.426(12) . ?
C3 H3D 0.9700 . ?
C3 H3E 0.9700 . ?
C5 H5C 0.9700 . ?
C5 H5D 0.9700 . ?
C5 C6 1.495(11) . ?
C6 H6D 0.9700 . ?
C6 H6E 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
I2 Ge1 I1 91.22(3) . . ?
I2 Ge1 I3 95.43(3) . . ?
I3 Ge1 I1 93.49(3) . . ?
I6 Ge2 I7 95.45(3) . . ?
I8 Ge2 I6 95.20(3) . . ?
I8 Ge2 I7 90.83(3) . . ?
C1 S1 C2 106.8(5) . . ?
C4 S2 C5 102.9(4) . . ?
H1A N1 H1B 120.0 . . ?
C1 N1 H1A 120.0 . . ?
C1 N1 H1B 120.0 . . ?
H2A N2 H2B 120.0 . . ?
C1 N2 H2A 120.0 . . ?
C1 N2 H2B 120.0 . . ?
H3A N3 H3B 109.5 . . ?
H3A N3 H3C 109.5 . . ?
H3B N3 H3C 109.5 . . ?
C3 N3 H3A 109.5 . . ?
C3 N3 H3B 109.5 . . ?
C3 N3 H3C 109.5 . . ?
H4A N4 H4B 120.0 . . ?
C4 N4 H4A 120.0 . . ?
C4 N4 H4B 120.0 . . ?
H5A N5 H5B 120.0 . . ?
C4 N5 H5A 120.0 . . ?
C4 N5 H5B 120.0 . . ?
H6A N6 H6B 109.5 . . ?
H6A N6 H6C 109.5 . . ?
H6B N6 H6C 109.5 . . ?
C6 N6 H6A 109.5 . . ?
C6 N6 H6B 109.5 . . ?
C6 N6 H6C 109.5 . . ?
N1 C1 S1 122.7(8) . . ?
N2 C1 S1 115.6(8) . . ?
N2 C1 N1 121.8(10) . . ?
S1 C2 H2C 109.5 . . ?
S1 C2 H2D 109.5 . . ?
H2C C2 H2D 108.1 . . ?
C3 C2 S1 110.9(6) . . ?
C3 C2 H2C 109.5 . . ?
C3 C2 H2D 109.5 . . ?
N3 C3 H3D 109.2 . . ?
N3 C3 H3E 109.2 . . ?
C2 C3 N3 112.1(7) . . ?
C2 C3 H3D 109.2 . . ?
C2 C3 H3E 109.2 . . ?
H3D C3 H3E 107.9 . . ?
N4 C4 S2 117.6(7) . . ?
N5 C4 S2 122.2(6) . . ?
N5 C4 N4 120.2(8) . . ?
S2 C5 H5C 109.7 . . ?
S2 C5 H5D 109.7 . . ?
H5C C5 H5D 108.2 . . ?
C6 C5 S2 109.7(6) . . ?
C6 C5 H5C 109.7 . . ?
C6 C5 H5D 109.7 . . ?
N6 C6 C5 112.6(7) . . ?
N6 C6 H6D 109.1 . . ?
N6 C6 H6E 109.1 . . ?
C5 C6 H6D 109.1 . . ?
C5 C6 H6E 109.1 . . ?
H6D C6 H6E 107.8 . . ?

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
S1 C2 C3 N3 -164.1(7) . . . . ?
S2 C5 C6 N6 -75.8(9) . . . . ?
C1 S1 C2 C3 -104.4(8) . . . . ?
C2 S1 C1 N1 6.3(9) . . . . ?
C2 S1 C1 N2 -172.7(9) . . . . ?
C4 S2 C5 C6 148.4(6) . . . . ?
C5 S2 C4 N4 -149.5(6) . . . . ?
C5 S2 C4 N5 34.0(8) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_a_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 2169494'
loop_
_audit_author_name
_audit_author_address
'Congcong Chen'
;Southern University of Science and Technology
China
;
_audit_update_record             
;
2022-04-29 deposited with the CCDC.	2022-08-05 downloaded from the CCDC.
;
_audit_creation_date             2022-02-16
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'I10 Sn2, I6 Sn2, 4(C3 H11 N3 S)'
_chemical_formula_sum            'C12 H44 I16 N12 S4 Sn4'
_chemical_formula_weight         2989.99
_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'
I I -0.4742 1.8119 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 '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           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   19.472(4)
_cell_length_b                   12.509(2)
_cell_length_c                   25.392(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6185.2(19)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2337
_cell_measurement_temperature    100.01
_cell_measurement_theta_max      21.77
_cell_measurement_theta_min      2.64
_shelx_estimated_absorpt_T_max   0.502
_shelx_estimated_absorpt_T_min   0.449
_exptl_absorpt_coefficient_mu    9.742
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4100
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    3.211
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             5248
_exptl_crystal_size_max          0.098
_exptl_crystal_size_mid          0.086
_exptl_crystal_size_min          0.082
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1319
_diffrn_reflns_av_unetI/netI     0.1243
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            30438
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.390
_diffrn_reflns_theta_min         1.604
_diffrn_ambient_temperature      100.01
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_voltage           40.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3177
_reflns_number_total             6325
_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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_refine_diff_density_max         1.272
_refine_diff_density_min         -1.648
_refine_diff_density_rms         0.275
_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     220
_refine_ls_number_reflns         6325
_refine_ls_number_restraints     103
_refine_ls_R_factor_all          0.1537
_refine_ls_R_factor_gt           0.0569
_refine_ls_restrained_S_all      1.029
_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)+(0.0339P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1046
_refine_ls_wR_factor_ref         0.1392
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups, All N(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
N6 \\sim S2 \\sim C5 \\sim C6 \\sim C4 \\sim H5C \\sim H5D \\sim N5 \\sim N4
\\sim H4D \\sim H4E \\sim H5A \\sim H5B \\sim H6A \\sim H6B \\sim H4A \\sim H4B
\\sim H4C: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
within 1.7A
3.a Rotating group:
 N3(H3A,H3B)
3.b Secondary CH2 refined with riding coordinates:
 C1(H1D,H1E), C2(H2C,H2D), C4(H4D,H4E), C5(H5C,H5D)
3.c X=CH2 refined with riding coordinates:
 N2(H2A,H2B), N5(H5A,H5B), N6(H6A,H6B)
3.d Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N4(H4A,H4B,H4C)
;
_atom_sites_solution_hydrogens   mixed
_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
I1 I 0.35904(6) 0.45379(10) 1.30878(5) 0.0632(4) Uani 1 1 d . . . . .
I2 I 0.51911(6) 0.20671(8) 1.27245(5) 0.0550(3) Uani 1 1 d . . . . .
I3 I 0.63308(6) 0.44901(9) 1.17916(4) 0.0497(3) Uani 1 1 d . . . . .
I4 I 0.41003(7) 0.40369(11) 1.15052(4) 0.0665(4) Uani 1 1 d . . . . .
Sn1 Sn 0.49504(5) 0.45338(8) 1.24546(4) 0.0333(3) Uani 1 1 d . . . . .
I5 I 0.58957(6) 0.51576(9) 1.34948(4) 0.0503(3) Uani 1 1 d . . . . .
I6 I 0.37732(6) 0.48298(9) 1.48333(4) 0.0542(3) Uani 1 1 d . . . . .
I7 I 0.23805(6) 0.70325(9) 1.40385(5) 0.0552(3) Uani 1 1 d . . . . .
I8 I 0.16038(6) 0.45051(9) 1.50464(4) 0.0496(3) Uani 1 1 d . . . . .
Sn2 Sn 0.25357(5) 0.45688(8) 1.41234(4) 0.0327(3) Uani 1 1 d . . . . .
S1 S 0.7746(3) 0.6940(4) 1.36164(18) 0.0652(14) Uani 1 1 d . . . . .
N1 N 0.6794(7) 0.6942(11) 1.2550(5) 0.063(4) Uani 1 1 d . . . . .
H1A H 0.668981 0.655817 1.225683 0.075 Uiso 1 1 calc R U . . .
H1B H 0.656689 0.757794 1.254180 0.075 Uiso 1 1 calc R U . . .
H1C H 0.666477 0.656931 1.284171 0.075 Uiso 1 1 calc R U . . .
N2 N 0.7671(7) 0.8820(13) 1.4101(5) 0.070(5) Uani 1 1 d . . . . .
H2A H 0.755006 0.922903 1.436722 0.084 Uiso 1 1 calc R U . . .
H2B H 0.792615 0.908215 1.384578 0.084 Uiso 1 1 calc R U . . .
N3 N 0.7092(9) 0.7427(14) 1.4465(6) 0.080(5) Uani 1 1 d . . . . .
H3A H 0.675892 0.704671 1.431129 0.096 Uiso 1 1 d R U . . .
H3B H 0.688448 0.791566 1.466981 0.096 Uiso 1 1 d R U . . .
C1 C 0.7552(9) 0.7143(14) 1.2569(7) 0.060(5) Uani 1 1 d . . . . .
H1D H 0.769028 0.752864 1.224508 0.073 Uiso 1 1 calc R U . . .
H1E H 0.779498 0.644765 1.257145 0.073 Uiso 1 1 calc R U . . .
C2 C 0.7774(9) 0.7780(14) 1.3039(5) 0.053(5) Uani 1 1 d . . . . .
H2C H 0.746442 0.840056 1.308625 0.064 Uiso 1 1 calc R U . . .
H2D H 0.824606 0.805062 1.298480 0.064 Uiso 1 1 calc R U . . .
C3 C 0.7479(8) 0.7856(15) 1.4085(6) 0.047(4) Uani 1 1 d . . . . .
S2 S 0.5380(3) 0.8204(4) 1.49209(18) 0.0596(13) Uani 1 1 d . U . . .
N4 N 0.4320(7) 0.6801(10) 1.3766(5) 0.064(4) Uani 1 1 d . U . . .
H4A H 0.403777 0.712819 1.353002 0.076 Uiso 1 1 calc R U . . .
H4B H 0.412683 0.617386 1.387177 0.076 Uiso 1 1 calc R U . . .
H4C H 0.473284 0.666669 1.361181 0.076 Uiso 1 1 calc R U . . .
N5 N 0.5264(12) 0.8660(19) 1.5889(7) 0.146(7) Uani 1 1 d . U . . .
H5A H 0.513107 0.854852 1.621576 0.175 Uiso 1 1 calc R U . . .
H5B H 0.548184 0.925290 1.580644 0.175 Uiso 1 1 calc R U . . .
N6 N 0.4820(12) 0.7137(17) 1.5708(8) 0.134(7) Uani 1 1 d . U . . .
H6A H 0.470163 0.707530 1.604138 0.160 Uiso 1 1 calc R U . . .
H6B H 0.471887 0.662403 1.548397 0.160 Uiso 1 1 calc R U . . .
C4 C 0.4419(10) 0.7494(16) 1.4221(7) 0.073(4) Uani 1 1 d . U . . .
H4D H 0.400964 0.745612 1.445135 0.088 Uiso 1 1 calc R U . . .
H4E H 0.447160 0.824278 1.410110 0.088 Uiso 1 1 calc R U . . .
C5 C 0.5045(11) 0.7164(16) 1.4526(8) 0.084(5) Uani 1 1 d . U . . .
H5C H 0.540371 0.692367 1.427670 0.101 Uiso 1 1 calc R U . . .
H5D H 0.492557 0.654998 1.475472 0.101 Uiso 1 1 calc R U . . .
C6 C 0.5145(12) 0.7986(17) 1.5547(8) 0.075(5) Uani 1 1 d . 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
I1 Sn1 3.0980(16) . ?
I2 Sn1 3.2133(15) 3_647 ?
I2 Sn1 3.1955(15) . ?
I3 Sn1 3.1721(15) . ?
I4 Sn1 2.9896(15) . ?
Sn1 I5 3.3128(15) . ?
I6 Sn2 3.0269(15) . ?
I7 Sn2 3.1042(16) . ?
I7 Sn2 3.1843(16) 8_665 ?
I8 Sn2 2.9653(15) . ?
S1 C2 1.805(16) . ?
S1 C3 1.732(18) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 H1C 0.9100 . ?
N1 C1 1.498(19) . ?
N2 H2A 0.8800 . ?
N2 H2B 0.8800 . ?
N2 C3 1.26(2) . ?
N3 H3A 0.8928 . ?
N3 H3B 0.8989 . ?
N3 C3 1.336(19) . ?
C1 H1D 0.9900 . ?
C1 H1E 0.9900 . ?
C1 C2 1.50(2) . ?
C2 H2C 0.9900 . ?
C2 H2D 0.9900 . ?
S2 C5 1.767(18) . ?
S2 C6 1.68(2) . ?
N4 H4A 0.9100 . ?
N4 H4B 0.9100 . ?
N4 H4C 0.9100 . ?
N4 C4 1.457(19) . ?
N5 H5A 0.8800 . ?
N5 H5B 0.8800 . ?
N5 C6 1.23(2) . ?
N6 H6A 0.8800 . ?
N6 H6B 0.8800 . ?
N6 C6 1.30(3) . ?
C4 H4D 0.9900 . ?
C4 H4E 0.9900 . ?
C4 C5 1.50(2) . ?
C5 H5C 0.9900 . ?
C5 H5D 0.9900 . ?

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
Sn1 I2 Sn1 155.42(4) . 3_647 ?
I1 Sn1 I2 89.92(4) . 3_657 ?
I1 Sn1 I2 90.90(4) . . ?
I1 Sn1 I3 178.80(5) . . ?
I1 Sn1 I5 93.49(4) . . ?
I2 Sn1 I2 174.43(4) . 3_657 ?
I2 Sn1 I5 88.56(4) . . ?
I2 Sn1 I5 85.89(4) 3_657 . ?
I3 Sn1 I2 88.45(4) . . ?
I3 Sn1 I2 90.83(4) . 3_657 ?
I3 Sn1 I5 87.50(4) . . ?
I4 Sn1 I1 86.88(5) . . ?
I4 Sn1 I2 93.06(4) . . ?
I4 Sn1 I2 92.49(4) . 3_657 ?
I4 Sn1 I3 92.16(4) . . ?
I4 Sn1 I5 178.33(5) . . ?
Sn2 I7 Sn2 168.39(5) . 8_665 ?
I6 Sn2 I7 96.14(4) . 8_655 ?
I6 Sn2 I7 90.68(4) . . ?
I7 Sn2 I7 171.70(5) . 8_655 ?
I8 Sn2 I6 91.11(4) . . ?
I8 Sn2 I7 93.33(4) . 8_655 ?
I8 Sn2 I7 91.26(4) . . ?
C3 S1 C2 100.5(9) . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
H2A N2 H2B 120.0 . . ?
C3 N2 H2A 120.0 . . ?
C3 N2 H2B 120.0 . . ?
H3A N3 H3B 106.8 . . ?
C3 N3 H3A 108.0 . . ?
C3 N3 H3B 113.4 . . ?
N1 C1 H1D 108.9 . . ?
N1 C1 H1E 108.9 . . ?
N1 C1 C2 113.4(13) . . ?
H1D C1 H1E 107.7 . . ?
C2 C1 H1D 108.9 . . ?
C2 C1 H1E 108.9 . . ?
S1 C2 H2C 109.8 . . ?
S1 C2 H2D 109.8 . . ?
C1 C2 S1 109.2(13) . . ?
C1 C2 H2C 109.8 . . ?
C1 C2 H2D 109.8 . . ?
H2C C2 H2D 108.3 . . ?
N2 C3 S1 124.3(13) . . ?
N2 C3 N3 121.9(17) . . ?
N3 C3 S1 113.6(15) . . ?
C6 S2 C5 108.5(11) . . ?
H4A N4 H4B 109.5 . . ?
H4A N4 H4C 109.5 . . ?
H4B N4 H4C 109.5 . . ?
C4 N4 H4A 109.5 . . ?
C4 N4 H4B 109.5 . . ?
C4 N4 H4C 109.5 . . ?
H5A N5 H5B 120.0 . . ?
C6 N5 H5A 120.0 . . ?
C6 N5 H5B 120.0 . . ?
H6A N6 H6B 120.0 . . ?
C6 N6 H6A 120.0 . . ?
C6 N6 H6B 120.0 . . ?
N4 C4 H4D 109.5 . . ?
N4 C4 H4E 109.5 . . ?
N4 C4 C5 110.7(16) . . ?
H4D C4 H4E 108.1 . . ?
C5 C4 H4D 109.5 . . ?
C5 C4 H4E 109.5 . . ?
S2 C5 H5C 109.0 . . ?
S2 C5 H5D 109.0 . . ?
C4 C5 S2 113.0(15) . . ?
C4 C5 H5C 109.0 . . ?
C4 C5 H5D 109.0 . . ?
H5C C5 H5D 107.8 . . ?
N5 C6 S2 120(2) . . ?
N5 C6 N6 115(2) . . ?
N6 C6 S2 124.3(17) . . ?

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 S1 74.4(17) . . . . ?
C2 S1 C3 N2 -37.8(18) . . . . ?
C2 S1 C3 N3 147.9(13) . . . . ?
C3 S1 C2 C1 -144.2(12) . . . . ?
N4 C4 C5 S2 158.0(14) . . . . ?
C5 S2 C6 N5 -173(2) . . . . ?
C5 S2 C6 N6 5(2) . . . . ?
C6 S2 C5 C4 102.5(17) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_a_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 2169493'
loop_
_audit_author_name
_audit_author_address
'Congcong Chen'
;Southern University of Science and Technology
China
;
_audit_update_record             
;
2022-04-29 deposited with the CCDC.	2022-08-05 downloaded from the CCDC.
;
_audit_creation_date             2022-02-16
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'I8 Pb2, 2(C3 H11 N3 S)'
_chemical_formula_sum            'C6 H22 I8 N6 Pb2 S2'
_chemical_formula_weight         1671.99
_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'
I I -0.4742 1.8119 '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'
S S 0.1246 0.1234 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   12.2987(6)
_cell_length_b                   12.5368(6)
_cell_length_c                   19.8230(10)
_cell_angle_alpha                90
_cell_angle_beta                 92.204(2)
_cell_angle_gamma                90
_cell_volume                     3054.2(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9926
_cell_measurement_temperature    99.93
_cell_measurement_theta_max      25.404
_cell_measurement_theta_min      2.563
_shelx_estimated_absorpt_T_max   0.244
_shelx_estimated_absorpt_T_min   0.212
_exptl_absorpt_coefficient_mu    19.240
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.1887
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1783 before and 0.1172 after correction.
The Ratio of minimum to maximum transmission is 0.2532.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    3.636
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.117
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.102
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0945
_diffrn_reflns_av_unetI/netI     0.0528
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            43292
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.390
_diffrn_reflns_theta_min         2.321
_diffrn_ambient_temperature      99.93
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5041
_reflns_number_total             5607
_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       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         6.990
_refine_diff_density_min         -10.756
_refine_diff_density_rms         0.955
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     165
_refine_ls_number_reflns         5607
_refine_ls_number_restraints     248
_refine_ls_R_factor_all          0.0779
_refine_ls_R_factor_gt           0.0713
_refine_ls_restrained_S_all      1.002
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1123P)²+336.3998P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1898
_refine_ls_wR_factor_ref         0.1962
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups, All N(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
S1 \\sim N1 \\sim H1A \\sim H1B \\sim N2 \\sim H2A \\sim H2B \\sim N3 \\sim H3A
\\sim H3B \\sim H3C \\sim C1 \\sim C2 \\sim H2C \\sim H2D \\sim C3 \\sim H3D
\\sim H3E: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
within 1.7A
S2 \\sim N4 \\sim N5 \\sim H5A \\sim H5B \\sim N6 \\sim H6A \\sim H6B \\sim H6C
\\sim C4 \\sim C5 \\sim H5C \\sim H5D \\sim C6 \\sim H6D \\sim H6E: within 1.7A
with sigma of 0.02 and sigma for terminal atoms of 0.04 within 1.7A
I1 \\sim Pb1 \\sim I4 \\sim I3 \\sim I5 \\sim I2 \\sim Pb2 \\sim I6 \\sim I7
\\sim I8: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
within 1.7A
H2C \\sim S1 \\sim C1 \\sim C2 \\sim N1 \\sim N2 \\sim H2D \\sim C3 \\sim H1A
\\sim H1B \\sim H2A \\sim H2B \\sim N3 \\sim H3D \\sim H3E \\sim H3A \\sim H3B
\\sim H3C \\sim H5D \\sim S2 \\sim C4 \\sim C5 \\sim N4 \\sim N5 \\sim H5C
\\sim C6 \\sim H4A \\sim H4B \\sim H5A \\sim H5B \\sim N6 \\sim H6D \\sim H6E
\\sim H6A \\sim H6B \\sim H6C: within 1.7A with sigma of 0.02 and sigma for
terminal atoms of 0.04 within 1.7A
Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(N3) \\sim
Ueq, Uanis(C3) \\sim Ueq, Uanis(S1) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
Uanis(C4) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(I1) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(I1) = Uanis(Pb1) = Uanis(I4) = Uanis(I3) = Uanis(I5) = Uanis(I2) =
Uanis(Pb2) = Uanis(I6) = Uanis(I7) = Uanis(I8)
3.a Secondary CH2 refined with riding coordinates:
 C2(H2C,H2D), C3(H3D,H3E), C5(H5C,H5D), C6(H6D,H6E)
3.b X=CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B), N4(H4A,H4B), N5(H5A,H5B)
3.c Idealised Me refined as rotating group:
 N3(H3A,H3B,H3C), N6(H6A,H6B,H6C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
Pb1 Pb 0.49460(5) 0.07064(6) 0.24799(3) 0.00642(18) Uani 1 1 d . . . . .
Pb2 Pb -0.00574(5) 0.06303(6) 0.25228(3) 0.00642(18) Uani 1 1 d . . . . .
I1 I 0.53498(9) 0.09129(9) 0.41018(6) 0.00642(18) Uani 1 1 d . U . . .
I2 I 0.74301(9) 0.12308(9) 0.21895(6) 0.00642(18) Uani 1 1 d . . . . .
I3 I 0.44456(10) 0.31893(9) 0.23861(6) 0.00642(18) Uani 1 1 d . . . . .
I4 I 0.44190(9) 0.04074(9) 0.09429(6) 0.00642(18) Uani 1 1 d . . . . .
I5 I 0.24743(9) 0.01469(9) 0.27750(6) 0.00642(18) Uani 1 1 d . . . . .
I6 I -0.03785(9) 0.02748(9) 0.40504(6) 0.00642(18) Uani 1 1 d . . . . .
I7 I -0.05370(10) -0.18317(9) 0.23431(6) 0.00642(18) Uani 1 1 d . . . . .
I8 I 0.03777(9) 0.08388(9) 0.09284(6) 0.00642(18) Uani 1 1 d . . . . .
S1 S 0.6922(4) 0.3176(4) 0.5141(2) 0.0080(9) Uani 1 1 d . U . . .
N1 N 0.6734(16) 0.1354(16) 0.5760(9) 0.022(4) Uani 1 1 d . U . . .
H1A H 0.696553 0.080843 0.600434 0.027 Uiso 1 1 calc R U . . .
H1B H 0.604074 0.140470 0.563544 0.027 Uiso 1 1 calc R U . . .
N2 N 0.8448(16) 0.1965(14) 0.5784(9) 0.018(4) Uani 1 1 d . U . . .
H2A H 0.866015 0.141195 0.602875 0.022 Uiso 1 1 calc R U . . .
H2B H 0.892376 0.245014 0.566980 0.022 Uiso 1 1 calc R U . . .
N3 N 0.7021(14) 0.3064(13) 0.3517(9) 0.014(3) Uani 1 1 d . U . . .
H3A H 0.715729 0.289359 0.308262 0.016 Uiso 1 1 calc R U . . .
H3B H 0.678788 0.375194 0.353730 0.016 Uiso 1 1 calc R U . . .
H3C H 0.649678 0.262319 0.367105 0.016 Uiso 1 1 calc R U . . .
C1 C 0.7398(17) 0.2069(17) 0.5586(11) 0.014(4) Uani 1 1 d . U . . .
C2 C 0.7998(18) 0.3545(18) 0.4600(11) 0.018(4) Uani 1 1 d . U . . .
H2C H 0.792988 0.431501 0.449632 0.021 Uiso 1 1 calc R U . . .
H2D H 0.870224 0.343891 0.484989 0.021 Uiso 1 1 calc R U . . .
C3 C 0.8027(18) 0.2939(17) 0.3942(11) 0.017(4) Uani 1 1 d . U . . .
H3D H 0.865273 0.319282 0.368639 0.020 Uiso 1 1 calc R U . . .
H3E H 0.814162 0.217271 0.404086 0.020 Uiso 1 1 calc R U . . .
S2 S 0.8361(4) 0.7601(4) 0.5508(2) 0.0079(9) Uani 1 1 d . . . . .
N4 N 0.6362(14) 0.6794(13) 0.5745(9) 0.012(3) Uani 1 1 d . U . . .
H4A H 0.591935 0.626507 0.583338 0.014 Uiso 1 1 calc R U . . .
H4B H 0.610180 0.744172 0.568072 0.014 Uiso 1 1 calc R U . . .
N5 N 0.7824(15) 0.5645(13) 0.5802(8) 0.013(3) Uani 1 1 d . U . . .
H5A H 0.738431 0.511330 0.589055 0.016 Uiso 1 1 calc R U . . .
H5B H 0.852682 0.552981 0.577601 0.016 Uiso 1 1 calc R U . . .
N6 N 0.7794(14) 0.8053(13) 0.3886(9) 0.012(3) Uani 1 1 d . U . . .
H6A H 0.743933 0.798764 0.347688 0.014 Uiso 1 1 calc R U . . .
H6B H 0.816056 0.743903 0.398567 0.014 Uiso 1 1 calc R U . . .
H6C H 0.827265 0.860536 0.387416 0.014 Uiso 1 1 calc R U . . .
C4 C 0.7428(14) 0.6614(14) 0.5706(9) 0.003(3) Uani 1 1 d . U . . .
C5 C 0.7527(15) 0.8586(15) 0.5075(9) 0.007(3) Uani 1 1 d . U . . .
H5C H 0.694552 0.880415 0.537779 0.008 Uiso 1 1 calc R U . . .
H5D H 0.798204 0.922248 0.499724 0.008 Uiso 1 1 calc R U . . .
C6 C 0.6999(15) 0.8259(15) 0.4408(10) 0.007(3) Uani 1 1 d . U . . .
H6D H 0.656261 0.760579 0.447379 0.009 Uiso 1 1 calc R U . . .
H6E H 0.649578 0.882991 0.424799 0.009 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 I1 3.2446(13) . ?
Pb1 I2 3.1988(13) . ?
Pb1 I3 3.1771(13) . ?
Pb1 I3 3.2516(13) 2_645 ?
Pb1 I4 3.1132(13) . ?
Pb1 I5 3.1956(13) . ?
Pb2 I2 3.2240(13) 1_455 ?
Pb2 I5 3.1926(13) . ?
Pb2 I6 3.1011(13) . ?
Pb2 I7 3.2734(13) 2 ?
Pb2 I7 3.1599(13) . ?
Pb2 I8 3.2364(13) . ?
S1 C1 1.73(2) . ?
S1 C2 1.80(2) . ?
N1 H1A 0.8800 . ?
N1 H1B 0.8800 . ?
N1 C1 1.27(3) . ?
N2 H2A 0.8800 . ?
N2 H2B 0.8800 . ?
N2 C1 1.34(3) . ?
N3 H3A 0.9100 . ?
N3 H3B 0.9100 . ?
N3 H3C 0.9100 . ?
N3 C3 1.48(3) . ?
C2 H2C 0.9900 . ?
C2 H2D 0.9900 . ?
C2 C3 1.51(3) . ?
C3 H3D 0.9900 . ?
C3 H3E 0.9900 . ?
S2 C4 1.743(18) . ?
S2 C5 1.802(19) . ?
N4 H4A 0.8800 . ?
N4 H4B 0.8800 . ?
N4 C4 1.34(3) . ?
N5 H5A 0.8800 . ?
N5 H5B 0.8800 . ?
N5 C4 1.32(2) . ?
N6 H6A 0.9100 . ?
N6 H6B 0.9100 . ?
N6 H6C 0.9100 . ?
N6 C6 1.47(3) . ?
C5 H5C 0.9900 . ?
C5 H5D 0.9900 . ?
C5 C6 1.51(3) . ?
C6 H6D 0.9900 . ?
C6 H6E 0.9900 . ?

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 I3 88.31(3) . 2_645 ?
I2 Pb1 I1 92.93(3) . . ?
I2 Pb1 I3 89.76(3) . 2_645 ?
I3 Pb1 I1 90.10(3) . . ?
I3 Pb1 I2 88.41(3) . . ?
I3 Pb1 I3 177.51(3) . 2_645 ?
I3 Pb1 I5 92.42(3) . . ?
I4 Pb1 I1 175.99(4) . . ?
I4 Pb1 I2 90.74(3) . . ?
I4 Pb1 I3 91.61(3) . . ?
I4 Pb1 I3 90.10(3) . 2_645 ?
I4 Pb1 I5 89.37(3) . . ?
I5 Pb1 I1 86.93(3) . . ?
I5 Pb1 I2 179.15(4) . . ?
I5 Pb1 I3 89.40(3) . 2_645 ?
I2 Pb2 I7 89.94(3) 1_455 2 ?
I2 Pb2 I8 88.52(3) 1_455 . ?
I5 Pb2 I2 176.12(4) . 1_455 ?
I5 Pb2 I7 87.61(3) . 2 ?
I5 Pb2 I8 88.36(3) . . ?
I6 Pb2 I2 94.40(3) . 1_455 ?
I6 Pb2 I5 88.84(3) . . ?
I6 Pb2 I7 95.56(3) . 2 ?
I6 Pb2 I7 86.53(3) . . ?
I6 Pb2 I8 175.79(4) . . ?
I7 Pb2 I2 91.82(3) . 1_455 ?
I7 Pb2 I5 90.51(3) . . ?
I7 Pb2 I7 177.16(2) . 2 ?
I7 Pb2 I8 90.34(3) . . ?
I8 Pb2 I7 87.48(3) . 2 ?
Pb1 I2 Pb2 146.06(4) . 1_655 ?
Pb1 I3 Pb1 154.50(4) . 2_655 ?
Pb2 I5 Pb1 149.16(4) . . ?
Pb2 I7 Pb2 154.18(4) . 2_545 ?
C1 S1 C2 105.5(10) . . ?
H1A N1 H1B 120.0 . . ?
C1 N1 H1A 120.0 . . ?
C1 N1 H1B 120.0 . . ?
H2A N2 H2B 120.0 . . ?
C1 N2 H2A 120.0 . . ?
C1 N2 H2B 120.0 . . ?
H3A N3 H3B 109.5 . . ?
H3A N3 H3C 109.5 . . ?
H3B N3 H3C 109.5 . . ?
C3 N3 H3A 109.5 . . ?
C3 N3 H3B 109.5 . . ?
C3 N3 H3C 109.5 . . ?
N1 C1 S1 119.7(17) . . ?
N1 C1 N2 118(2) . . ?
N2 C1 S1 121.9(16) . . ?
S1 C2 H2C 108.4 . . ?
S1 C2 H2D 108.4 . . ?
H2C C2 H2D 107.5 . . ?
C3 C2 S1 115.4(16) . . ?
C3 C2 H2C 108.4 . . ?
C3 C2 H2D 108.4 . . ?
N3 C3 C2 113.1(18) . . ?
N3 C3 H3D 109.0 . . ?
N3 C3 H3E 109.0 . . ?
C2 C3 H3D 109.0 . . ?
C2 C3 H3E 109.0 . . ?
H3D C3 H3E 107.8 . . ?
C4 S2 C5 103.1(9) . . ?
H4A N4 H4B 120.0 . . ?
C4 N4 H4A 120.0 . . ?
C4 N4 H4B 120.0 . . ?
H5A N5 H5B 120.0 . . ?
C4 N5 H5A 120.0 . . ?
C4 N5 H5B 120.0 . . ?
H6A N6 H6B 109.5 . . ?
H6A N6 H6C 109.5 . . ?
H6B N6 H6C 109.5 . . ?
C6 N6 H6A 109.5 . . ?
C6 N6 H6B 109.5 . . ?
C6 N6 H6C 109.5 . . ?
N4 C4 S2 123.3(14) . . ?
N5 C4 S2 116.4(14) . . ?
N5 C4 N4 120.3(17) . . ?
S2 C5 H5C 108.1 . . ?
S2 C5 H5D 108.1 . . ?
H5C C5 H5D 107.3 . . ?
C6 C5 S2 116.8(13) . . ?
C6 C5 H5C 108.1 . . ?
C6 C5 H5D 108.1 . . ?
N6 C6 C5 112.8(16) . . ?
N6 C6 H6D 109.0 . . ?
N6 C6 H6E 109.0 . . ?
C5 C6 H6D 109.0 . . ?
C5 C6 H6E 109.0 . . ?
H6D C6 H6E 107.8 . . ?

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
S1 C2 C3 N3 60(2) . . . . ?
C1 S1 C2 C3 83.6(17) . . . . ?
C2 S1 C1 N1 -147.8(18) . . . . ?
C2 S1 C1 N2 36(2) . . . . ?
S2 C5 C6 N6 -65.5(19) . . . . ?
C4 S2 C5 C6 -65.4(16) . . . . ?
C5 S2 C4 N4 -21.9(18) . . . . ?
C5 S2 C4 N5 156.2(15) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'