# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2023

####################################################################### 
# 
# 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_(MSBA)PbI4
_database_code_depnum_ccdc_archive 'CCDC 2249121'
loop_
_audit_author_name
_audit_author_address
'Wenxuan Li'
;Sun Yat sen University
China
;
_audit_update_record             
;
2023-03-16 deposited with the CCDC.	2023-10-02 downloaded from the CCDC.
;
_audit_creation_date             2022-11-12
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_chemical_formula_moiety         '0.5(I8 Pb2), C5 H16 N2 S2'
_chemical_formula_sum            'C5 H16 I4 N2 Pb S2'
_chemical_formula_weight         883.16
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
C 0.01920 0.00962 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
I -0.19193 6.94384 20.14720 18.99490 7.51380 2.27350 4.34700 0.38140 27.76600
66.87760 4.07119989395
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.03256 0.01839 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.5290002823
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Pb -3.72549 8.94614 31.06170 13.06370 18.44200 5.96960 0.69020 2.35760 8.61800
47.25790 13.4118003845
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
S 0.33536 0.55132 6.90530 5.20340 1.43790 1.58630 1.46790 22.21510 0.25360
56.17200 0.866900026798
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,y,-z+1/2
3 -x,-y,-z
4 x,-y,z-1/2
5 x+1/2,y+1/2,z
6 -x+1/2,y+1/2,-z+1/2
7 -x+1/2,-y+1/2,-z
8 x+1/2,-y+1/2,z-1/2

_symmetry_Int_Tables_number      15
_cell_length_a                   25.2413(6)
_cell_length_b                   8.7370(2)
_cell_length_c                   8.6774(2)
_cell_angle_alpha                90
_cell_angle_beta                 102.882(2)
_cell_angle_gamma                90
_cell_volume                     1865.49(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4424
_cell_measurement_temperature    149.98(10)
_cell_measurement_theta_max      0.124
_cell_measurement_theta_min      0.07122
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    71.485
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.07122
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.1443
_exptl_crystal_description       plate
_exptl_crystal_F_000             1536.5959
_exptl_crystal_preparation       ?
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            6053
_diffrn_reflns_theta_full        66.563
_diffrn_reflns_theta_max         66.563
_diffrn_reflns_theta_min         3.592
_diffrn_ambient_temperature      149.98(10)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              29
_reflns_limit_h_min              -30
_reflns_limit_k_max              10
_reflns_limit_k_min              0
_reflns_limit_l_max              10
_reflns_limit_l_min              0
_reflns_number_gt                1571
_reflns_number_total             1653
_reflns_threshold_expression     I>=2u(I)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         2.0866
_refine_diff_density_min         -2.3944
_refine_diff_density_rms         0.4066
_refine_ls_d_res_high            0.8402
_refine_ls_d_res_low             12.3030
_refine_ls_goodness_of_fit_ref   1.0233
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    13
_refine_ls_number_parameters     67
_refine_ls_number_reflns         1653
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0385
_refine_ls_restrained_S_all      1.0233
_refine_ls_shift/su_max          0.0007
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0730P)²+5.0243P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0970
_refine_ls_wR_factor_ref         0.0989
_olex2_refinement_description    
;
1. Others
 Fixed Sof: H3a(0.5) H3b(0.5)
2.a Secondary CH2 refined with riding coordinates:
 C1(H1d,H1e), C2(H2a,H2b), C3(H3a,H3b)
2.b Idealised Me refined as rotating group:
 N1(H1a,H1b,H1c)
;
_atom_sites_solution_primary     iterative
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_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Pb1 Pb 0.75 0.25 0.5 0.01097(17) Uani 1.000000 2 S T P
I1 I 0.620448(17) 0.27463(6) 0.40041(6) 0.01944(19) Uani 1.000000 1 . . .
I2 I 0.754323(17) 0.55855(5) 0.31231(5) 0.01778(18) Uani 1.000000 1 . . .
S1 S 0.51867(10) 0.7113(5) 0.4283(4) 0.0548(8) Uani 1.000000 1 . . .
N1 N 0.6445(3) 0.6686(9) 0.5053(9) 0.0257(15) Uani 1.000000 1 . . .
H1a H 0.632(2) 0.5736(18) 0.486(4) 0.0308(18) Uiso 1.000000 1 GR . .
H1b H 0.6804(3) 0.669(6) 0.518(5) 0.0308(18) Uiso 1.000000 1 GR . .
H1c H 0.636(2) 0.703(4) 0.5932(17) 0.0308(18) Uiso 1.000000 1 GR . .
C1 C 0.6196(4) 0.7698(13) 0.3703(14) 0.040(3) Uani 1.000000 1 . . .
H1d H 0.6454(4) 0.8488(13) 0.3592(14) 0.048(3) Uiso 1.000000 1 R . .
H1e H 0.6120(4) 0.7099(13) 0.2738(14) 0.048(3) Uiso 1.000000 1 R . .
C2 C 0.5685(4) 0.8430(12) 0.3907(15) 0.045(3) Uani 1.000000 1 . . .
H2a H 0.5529(4) 0.9007(12) 0.2958(15) 0.054(3) Uiso 1.000000 1 R . .
H2b H 0.5772(4) 0.9150(12) 0.4778(15) 0.054(3) Uiso 1.000000 1 R . .
C3 C 0.5 0.6058(18) 0.25 0.053(5) Uani 1.000000 2 S T P
H3a H 0.530239366098 0.5399(18) 0.242300433913 0.064(6) Uiso 0.500000 1 R . .
H3b H 0.469760633902 0.5399(18) 0.257699566087 0.064(6) Uiso 0.500000 1 R . .


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 3.1979(4) 7_656 ?
Pb1 I1 3.1979(4) . ?
Pb1 I2 3.1658(4) 4_566 ?
Pb1 I2 3.1640(4) 7_656 ?
Pb1 I2 3.1640(4) . ?
Pb1 I2 3.1658(4) 6_645 ?
S1 C2 1.788(11) . ?
S1 C3 1.772(9) . ?
N1 H1a 0.8900 . ?
N1 H1b 0.8900 . ?
N1 H1c 0.8900 . ?
N1 C1 1.490(12) . ?
C1 H1d 0.9700 . ?
C1 H1e 0.9700 . ?
C1 C2 1.484(15) . ?
C2 H2a 0.9700 . ?
C2 H2b 0.9700 . ?
C3 H3a 0.9700 . ?
C3 H3a 0.9700 2_655 ?
C3 H3b 0.9700 2_655 ?
C3 H3b 0.9700 . ?
H3a H3b 0.0000 2_655 ?

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 180.0 7_656 . ?
I2 Pb1 I1 87.370(12) . . ?
I2 Pb1 I1 92.630(12) . 7_656 ?
I2 Pb1 I1 92.630(12) 7_656 . ?
I2 Pb1 I1 87.370(12) 7_656 7_656 ?
I2 Pb1 I1 88.064(12) 6_645 . ?
I2 Pb1 I1 88.064(12) 4_566 7_656 ?
I2 Pb1 I1 91.936(12) 6_645 7_656 ?
I2 Pb1 I1 91.936(12) 4_566 . ?
I2 Pb1 I2 180.0 4_566 6_645 ?
I2 Pb1 I2 89.536(4) 4_566 . ?
I2 Pb1 I2 89.536(5) 7_656 6_645 ?
I2 Pb1 I2 180.0 7_656 . ?
C3 S1 C2 103.7(5) . . ?
H1b N1 H1a 109.5 . . ?
H1c N1 H1a 109.5 . . ?
H1c N1 H1b 109.5 . . ?
C1 N1 H1a 109.5 . . ?
C1 N1 H1b 109.5 . . ?
C1 N1 H1c 109.5 . . ?
H1d C1 N1 109.0(5) . . ?
H1e C1 N1 109.0(6) . . ?
H1e C1 H1d 107.8 . . ?
C2 C1 N1 112.8(9) . . ?
C2 C1 H1d 109.0(6) . . ?
C2 C1 H1e 109.0(6) . . ?
C1 C2 S1 114.1(8) . . ?
H2a C2 S1 108.7(4) . . ?
H2a C2 C1 108.7(6) . . ?
H2b C2 S1 108.7(4) . . ?
H2b C2 C1 108.7(6) . . ?
H2b C2 H2a 107.6 . . ?
S1 C3 S1 117.3(9) 2_655 . ?
H3a C3 S1 108.0(3) . . ?
H3a C3 S1 108.0(3) . 2_655 ?
H3a C3 S1 108.0(3) 2_655 . ?
H3a C3 S1 108.0(3) 2_655 2_655 ?
H3a C3 H3a 107.2 2_655 . ?
H3b C3 S1 108.0(3) 2_655 . ?
H3b C3 S1 108.0(3) 2_655 2_655 ?
H3b C3 S1 108.0(3) . . ?
H3b C3 S1 108.0(3) . 2_655 ?
H3b C3 H3a 107.2 2_655 2_655 ?
H3b C3 H3a 0.0 . 2_655 ?
H3b C3 H3a 107.2 . . ?
H3b C3 H3a 0.0 2_655 . ?
H3b C3 H3b 107.22989637(2) . 2_655 ?
H3b H3a C3 0(2200000) 2_655 . ?
H3a H3b C3 0(2000000) 2_655 2_655 ?

_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_(MSBA)(MA)Pb2I7
_database_code_depnum_ccdc_archive 'CCDC 2249140'
loop_
_audit_author_name
_audit_author_address
'Wenxuan Li'
;Sun Yat sen University
China
;
_audit_update_record             
;
2023-03-16 deposited with the CCDC.	2023-10-02 downloaded from the CCDC.
;
_audit_creation_date             2022-11-12
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'I7 Pb2, C5 H16 N2 S2, C H6 N'
_chemical_formula_sum            'C6 H22 I7 N3 Pb2 S2'
_chemical_formula_weight         1503.06
_chemical_melting_point          ?
_chemical_oxdiff_formula         C5I7N2Pb2S2
_chemical_oxdiff_usercomment     LWX-3
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           13
_space_group_name_H-M_alt        'P 1 2/c 1'
_space_group_name_Hall           '-P 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'

_cell_length_a                   18.6002(15)
_cell_length_b                   8.7989(4)
_cell_length_c                   8.7446(5)
_cell_angle_alpha                90
_cell_angle_beta                 94.801(6)
_cell_angle_gamma                90
_cell_volume                     1426.13(16)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4432
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      31.8910
_cell_measurement_theta_min      3.3710
_shelx_estimated_absorpt_T_max   0.758
_shelx_estimated_absorpt_T_min   0.387
_exptl_absorpt_coefficient_mu    19.510
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.35926
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    3.500
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1292
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.015
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_av_unetI/netI     0.0435
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            11584
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         3.072
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2913
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -102.00 -66.00   1.00   35.00    --  -18.80-178.00 -30.00   36
  2  ω    -40.00   7.00   1.00   35.00    --  -18.80 -77.00 150.00   47
  3  ω     -2.00  77.00   1.00   35.00    --   20.05  38.00-180.00   79
  4  ω     40.00  94.00   1.00   35.00    --   20.05 178.00-150.00   54
  5  ω     -4.00  94.00   1.00   35.00    --   20.05  38.00  30.00   98
  6  ω    -45.00  44.00   1.00   35.00    --   20.05 -38.00-150.00   89
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0002761000
_diffrn_orient_matrix_UB_12      -0.0222168000
_diffrn_orient_matrix_UB_13      -0.0780407000
_diffrn_orient_matrix_UB_21      -0.0343595000
_diffrn_orient_matrix_UB_22      0.0342635000
_diffrn_orient_matrix_UB_23      -0.0154139000
_diffrn_orient_matrix_UB_31      0.0168169000
_diffrn_orient_matrix_UB_32      0.0695119000
_diffrn_orient_matrix_UB_33      -0.0173428000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2222
_reflns_number_total             2527
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         8.517
_refine_diff_density_min         -1.867
_refine_diff_density_rms         0.506
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     104
_refine_ls_number_reflns         2527
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0767
_refine_ls_R_factor_gt           0.0685
_refine_ls_restrained_S_all      1.087
_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)+(0.1007P)²+103.6112P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1903
_refine_ls_wR_factor_ref         0.1972
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.93839
 0.06161
2. Restrained distances
 C7-N15
 1.49 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C7) \\sim Ueq, Uanis(N15) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Fixed Sof: H21A(0.5) H21B(0.5) N15(0.5) H15A(0.5) H15B(0.5) H15C(0.5) C7(0.5)
 H7A(0.5) H7B(0.5) H7C(0.5)
5.a Riding coordinates:
 N15(H15A,H15B,H15C)
5.b Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C21(H21A,H21B), C12(H12A,H12B)
5.c Idealised Me refined as rotating group:
 N8(H8A,H8B,H8C), C7(H7A,H7B,H7C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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 0.5000 0.7438(2) 0.7500 0.0246(5) Uani 1 2 d S T P . .
Pb2 Pb 0.67675(5) 0.74626(8) 0.78031(9) 0.0156(3) Uani 1 1 d . . . . .
I3 I 0.84417(9) 0.77627(17) 0.79342(19) 0.0255(4) Uani 1 1 d . . . . .
I4 I 0.67609(11) 0.55578(18) 0.47505(19) 0.0333(5) Uani 1 1 d . . . . .
I6 I 0.66654(9) 1.05068(16) 0.58012(16) 0.0228(4) Uani 1 1 d . . . . .
S1 S 0.9744(5) 0.7881(13) 0.4105(10) 0.060(3) Uani 1 1 d . . . . .
C19 C 0.9074(15) 0.658(3) 0.325(4) 0.047(8) Uani 1 1 d . . . . .
H19A H 0.9298 0.5916 0.2544 0.057 Uiso 1 1 calc R U . . .
H19B H 0.8903 0.5942 0.4057 0.057 Uiso 1 1 calc R U . . .
C21 C 1.0000 0.887(5) 0.2500 0.057(14) Uani 1 2 d S T P . .
H21A H 1.0399 0.9528 0.2849 0.068 Uiso 0.5 1 calc R U P . .
H21B H 0.9601 0.9528 0.2151 0.068 Uiso 0.5 1 calc R U P . .
N8 N 0.8070(13) 0.828(3) 0.370(2) 0.035(5) Uani 1 1 d . . . . .
H8A H 0.8232 0.7922 0.4613 0.042 Uiso 1 1 calc R U . . .
H8B H 0.7593 0.8180 0.3572 0.042 Uiso 1 1 calc R U . . .
H8C H 0.8184 0.9264 0.3640 0.042 Uiso 1 1 calc R U . . .
C12 C 0.8426(17) 0.737(4) 0.240(5) 0.065(13) Uani 1 1 d . . . . .
H12A H 0.8091 0.6641 0.1916 0.078 Uiso 1 1 calc R U . . .
H12B H 0.8582 0.8058 0.1622 0.078 Uiso 1 1 calc R U . . .
N15 N 0.474(5) 0.708(10) 0.271(14) 0.14(4) Uani 0.5 1 d D U P A -1
H15A H 0.4298 0.7241 0.2263 0.172 Uiso 0.5 1 d R U P A -1
H15B H 0.4744 0.6215 0.3239 0.172 Uiso 0.5 1 d R U P A -1
H15C H 0.5053 0.7025 0.2002 0.172 Uiso 0.5 1 d R U P A -1
C7 C 0.522(4) 0.830(7) 0.340(8) 0.054(17) Uani 0.5 1 d D U P A -1
H7A H 0.5085 0.8527 0.4416 0.081 Uiso 0.5 1 calc R U P A -1
H7B H 0.5169 0.9193 0.2778 0.081 Uiso 0.5 1 calc R U P A -1
H7C H 0.5710 0.7956 0.3464 0.081 Uiso 0.5 1 calc R U P A -1


_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 Pb2 3.2761(9) . ?
I1 Pb2 3.2761(9) 2_656 ?
Pb2 I3 3.1179(18) . ?
Pb2 I4 3.1511(16) . ?
Pb2 I4 3.1569(16) 4_566 ?
Pb2 I6 3.1914(15) 4_576 ?
Pb2 I6 3.1968(15) . ?
I4 Pb2 3.1569(16) 4_565 ?
I6 Pb2 3.1914(15) 4_575 ?
S1 C19 1.81(3) . ?
S1 C21 1.75(2) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C12 1.53(5) . ?
C21 S1 1.75(2) 2_755 ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
N8 H8A 0.8900 . ?
N8 H8B 0.8900 . ?
N8 H8C 0.8900 . ?
N8 C12 1.58(3) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
N15 H15A 0.8898 . ?
N15 H15B 0.8901 . ?
N15 H15C 0.8901 . ?
N15 C7 1.488(10) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 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
Pb2 I1 Pb2 179.25(8) . 2_656 ?
I3 Pb2 I1 174.86(5) . . ?
I3 Pb2 I4 90.53(5) . . ?
I3 Pb2 I4 95.76(5) . 4_566 ?
I3 Pb2 I6 87.85(5) . . ?
I3 Pb2 I6 92.88(5) . 4_576 ?
I4 Pb2 I1 89.37(5) 4_566 . ?
I4 Pb2 I1 89.73(5) . . ?
I4 Pb2 I4 90.53(2) . 4_566 ?
I4 Pb2 I6 176.38(5) 4_566 . ?
I4 Pb2 I6 91.43(4) 4_566 4_576 ?
I4 Pb2 I6 175.88(5) . 4_576 ?
I4 Pb2 I6 89.19(4) . . ?
I6 Pb2 I1 87.02(5) . . ?
I6 Pb2 I1 86.67(4) 4_576 . ?
I6 Pb2 I6 88.62(2) 4_576 . ?
Pb2 I4 Pb2 154.79(6) . 4_565 ?
Pb2 I6 Pb2 156.07(6) 4_575 . ?
C21 S1 C19 102.2(14) . . ?
S1 C19 H19A 108.9 . . ?
S1 C19 H19B 108.9 . . ?
H19A C19 H19B 107.7 . . ?
C12 C19 S1 113(2) . . ?
C12 C19 H19A 108.9 . . ?
C12 C19 H19B 108.9 . . ?
S1 C21 S1 120(3) . 2_755 ?
S1 C21 H21A 107.2 . . ?
S1 C21 H21A 107.2 2_755 . ?
S1 C21 H21B 107.2 . . ?
S1 C21 H21B 107.2 2_755 . ?
H21A C21 H21B 106.9 . . ?
H8A N8 H8B 109.5 . . ?
H8A N8 H8C 109.5 . . ?
H8B N8 H8C 109.5 . . ?
C12 N8 H8A 109.5 . . ?
C12 N8 H8B 109.5 . . ?
C12 N8 H8C 109.5 . . ?
C19 C12 N8 104(3) . . ?
C19 C12 H12A 111.0 . . ?
C19 C12 H12B 111.0 . . ?
N8 C12 H12A 111.0 . . ?
N8 C12 H12B 111.0 . . ?
H12A C12 H12B 109.0 . . ?
H15A N15 H15B 109.5 . . ?
H15A N15 H15C 109.5 . . ?
H15B N15 H15C 109.4 . . ?
C7 N15 H15A 124.4 . . ?
C7 N15 H15B 115.2 . . ?
C7 N15 H15C 85.3 . . ?
N15 C7 H7A 109.5 . . ?
N15 C7 H7B 109.5 . . ?
N15 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?

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 C19 C12 N8 -64(3) . . . . ?
C19 S1 C21 S1 -51.3(10) . . . 2_755 ?
C21 S1 C19 C12 -60(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.976
_oxdiff_exptl_absorpt_empirical_full_min 0.299
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.93839
2 0.06161

####################################################################### 
# 
# 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_(PDSBA)(MA)Pb2I7
_database_code_depnum_ccdc_archive 'CCDC 2249142'
loop_
_audit_author_name
_audit_author_address
'Wenxuan Li'
;Sun Yat sen University
China
;
_audit_update_record             
;
2023-03-16 deposited with the CCDC.	2023-10-02 downloaded from the CCDC.
;
_audit_creation_date             2022-11-12
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'I7 Pb2, C7 H20 N2 S2, C H6 N'
_chemical_formula_sum            'C8 H26 I7 N3 Pb2 S2'
_chemical_formula_weight         1531.12
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C40 H64 I28 N8 O4 Pb8 S8 '
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -4.0753 8.5060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   8.6911(2)
_cell_length_b                   8.7395(2)
_cell_length_c                   39.8628(14)
_cell_angle_alpha                90
_cell_angle_beta                 91.903(3)
_cell_angle_gamma                90
_cell_volume                     3026.14(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6648
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.2080
_cell_measurement_theta_min      6.0630
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    78.740
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.15392
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    3.361
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2648
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0679
_diffrn_reflns_av_unetI/netI     0.0567
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            24399
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        66.594
_diffrn_reflns_theta_max         66.594
_diffrn_reflns_theta_min         2.218
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     31.00  62.00   0.50    1.00    --    0.00  57.00 144.00   62
  2  ω     -3.00  23.00   0.50    1.00    --    0.00  57.00 144.00   52
  3  ω     79.00 185.00   0.50    3.00    --   95.80  57.00 144.00  212
  4  ω     41.00 118.00   0.50    3.00    --   95.80 -57.00   3.00  154
  5  ω    -32.00  30.00   0.50    1.00    --    0.00 -82.00  90.00  124
  6  ω     -1.00  85.00   0.50    1.00    --    0.00  38.00-120.00  172
  7  ω    -52.00 -11.00   0.50    1.00    --    0.00 -57.00   3.00   82
  8  ω    -30.00  24.00   0.50    1.00    --    0.00 -82.00 150.00  108
  9  ω     76.00 153.00   0.50    3.00    --   95.80  45.00-180.00  154
 10  ω     10.00 126.00   0.50    3.00    --   95.80 -82.00-150.00  232
 11  ω     32.00  67.00   0.50    3.00    --   95.80 -82.00 120.00   70
 12  ω     79.00 105.00   0.50    3.00    --   95.80 -82.00 -30.00   52
 13  ω     52.00 109.00   0.50    3.00    --   95.80 -30.00-150.00  114
 14  ω     94.00 124.00   0.50    3.00    --   95.80 -82.00-120.00   60
 15  ω     79.00 179.00   0.50    3.00    --   95.80  30.00  90.00  200
 16  ω     93.00 122.00   0.50    3.00    --   95.80 -82.00 -90.00   58
 17  ω     91.00 116.00   0.50    3.00    --   95.80 -82.00  60.00   50
 18  ω     79.00 136.00   0.50    3.00    --   95.80  45.00   0.00  114
 19  ω     49.00 127.00   0.50    3.00    --   95.80 -82.00  30.00  156
 20  ω     47.00  99.00   0.50    3.00    --   95.80 -82.00-180.00  104
 21  ω     82.00  87.50   0.50    3.00    --   95.80  30.00  60.00   11
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1031785000
_diffrn_orient_matrix_UB_12      -0.1388317000
_diffrn_orient_matrix_UB_13      0.0071006000
_diffrn_orient_matrix_UB_21      -0.0891443000
_diffrn_orient_matrix_UB_22      0.0959220000
_diffrn_orient_matrix_UB_23      0.0253239000
_diffrn_orient_matrix_UB_31      -0.1132976000
_diffrn_orient_matrix_UB_32      0.0509125000
_diffrn_orient_matrix_UB_33      -0.0283722000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3255
_reflns_number_total             5641
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         5.106
_refine_diff_density_min         -3.793
_refine_diff_density_rms         0.796
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.252
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         5641
_refine_ls_number_restraints     74
_refine_ls_R_factor_all          0.1825
_refine_ls_R_factor_gt           0.1423
_refine_ls_restrained_S_all      1.249
_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)+1924.9015P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3179
_refine_ls_wR_factor_ref         0.3320
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.96108
 0.03892
2. Restrained distances
 HB-H3A
 2.1 with sigma of 0.02
 HA_$1-H11A
 1.9 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq, Uanis(N00D) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C) \\sim
Ueq, Uanis(C3) \\sim Ueq, Uanis(N28) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C4)
\\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(I009) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(I009) \\sim Ueq, Uanis(N28) \\sim Ueq, Uanis(I003) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.01
Uanis(C11A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C4) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C32(H32A,H32B), C18(H18A,H18B)
4.b Idealised Me refined as rotating group:
 N00D(H00A,H00B,H00C), N28(H28A,H28B,H28C), C4(H4A,H4B,H4C), N1(H1C,H1D,H1E),
 C(HA,HB,HC), C11A(H11A,H11B,H11C)
;
_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
Pb01 Pb 0.2618(2) 0.75517(18) 0.58216(4) 0.0133(4) Uani 1 1 d . . . . .
Pb02 Pb 0.7620(2) 1.24335(18) 0.58222(4) 0.0131(4) Uani 1 1 d . . . . .
I003 I -0.0413(3) 0.5504(3) 0.57911(8) 0.0180(6) Uani 1 1 d . U . . .
I004 I 0.4573(3) 0.4441(3) 0.57912(8) 0.0167(6) Uani 1 1 d . . . . .
I005 I 0.2874(3) 0.7318(3) 0.66029(7) 0.0211(7) Uani 1 1 d . . . . .
I006 I 0.2484(4) 0.7541(3) 0.49989(9) 0.0224(6) Uani 1 1 d . . . . .
I007 I 0.7852(4) 1.2663(4) 0.66022(7) 0.0223(7) Uani 1 1 d . . . . .
I008 I 0.0749(4) 1.0621(3) 0.58099(9) 0.0291(8) Uani 1 1 d . . . . .
I009 I 0.5743(4) 0.9372(4) 0.58087(9) 0.0304(8) Uani 1 1 d . U . . .
S00B S 0.8138(19) 0.848(3) 0.7788(4) 0.059(5) Uani 1 1 d . . . . .
N00D N 0.791(6) 0.814(6) 0.8562(12) 0.040(10) Uani 1 1 d . U . . .
H00A H 0.8779 0.8408 0.8466 0.048 Uiso 1 1 calc R U . . .
H00B H 0.8126 0.7705 0.8760 0.048 Uiso 1 1 calc R U . . .
H00C H 0.7327 0.8961 0.8591 0.048 Uiso 1 1 calc R U . . .
C1 C 0.710(5) 0.707(5) 0.8351(11) 0.018(7) Uani 1 1 d . U . . .
H1A H 0.6108 0.7523 0.8290 0.022 Uiso 1 1 calc R U . . .
H1B H 0.6896 0.6171 0.8485 0.022 Uiso 1 1 calc R U . . .
S40 S 0.6897(16) 0.652(2) 0.7217(3) 0.038(4) Uani 1 1 d . . . . .
N28 N 0.705(4) 0.663(4) 0.6444(9) 0.018(6) Uani 1 1 d . U . . .
H28A H 0.7367 0.6602 0.6234 0.021 Uiso 1 1 calc R U . . .
H28B H 0.6115 0.7042 0.6447 0.021 Uiso 1 1 calc R U . . .
H28C H 0.7020 0.5683 0.6526 0.021 Uiso 1 1 calc R U . . .
C3 C 0.808(3) 0.752(4) 0.6643(6) 0.016(7) Uani 1 1 d . U . . .
H3A H 0.7675 0.8549 0.6662 0.019 Uiso 1 1 calc DR U . . .
H3B H 0.9060 0.7585 0.6534 0.019 Uiso 1 1 calc R U . . .
C9 C 0.641(6) 0.801(6) 0.7503(14) 0.030(8) Uani 1 1 d . U . . .
C32 C 0.780(6) 0.658(6) 0.8049(15) 0.036(14) Uani 1 1 d . . . . .
H32A H 0.7119 0.5884 0.7924 0.044 Uiso 1 1 calc R U . . .
H32B H 0.8763 0.6061 0.8099 0.044 Uiso 1 1 calc R U . . .
C18 C 0.832(7) 0.685(8) 0.6982(16) 0.046(8) Uani 1 1 d . U . . .
H18A H 0.9019 0.7530 0.7106 0.056 Uiso 1 1 calc R U . . .
H18B H 0.8865 0.5893 0.6955 0.056 Uiso 1 1 calc R U . . .
C4 C 0.829(6) 0.659(6) 0.4944(13) 0.028(8) Uani 1 1 d . U . . .
H4A H 0.8030 0.5910 0.4763 0.042 Uiso 1 1 calc R U . . .
H4B H 0.8531 0.6015 0.5143 0.042 Uiso 1 1 calc R U . . .
H4C H 0.9169 0.7197 0.4887 0.042 Uiso 1 1 calc R U . . .
N1 N 0.686(5) 0.771(5) 0.5009(11) 0.033(10) Uani 1 1 d . U . . .
H1C H 0.6200 0.7672 0.4834 0.040 Uiso 1 1 calc R U . . .
H1D H 0.7195 0.8661 0.5038 0.040 Uiso 1 1 calc R U . . .
H1E H 0.6386 0.7402 0.5193 0.040 Uiso 1 1 calc R U . . .
C C 0.633(3) 0.940(3) 0.7277(6) 0.030(11) Uani 1 1 d . U . . .
HA H 0.5486 1.0034 0.7340 0.045 Uiso 1 1 calc R U . . .
HB H 0.6176 0.9075 0.7048 0.045 Uiso 1 1 calc DR U . . .
HC H 0.7273 0.9964 0.7300 0.045 Uiso 1 1 calc R U . . .
C11A C 0.482(6) 0.764(3) 0.7682(11) 0.047(13) Uani 1 1 d . U . . .
H11A H 0.5010 0.6942 0.7865 0.071 Uiso 1 1 calc DR U . . .
H11B H 0.4108 0.7179 0.7522 0.071 Uiso 1 1 calc R U . . .
H11C H 0.4386 0.8568 0.7765 0.071 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
Pb01 I003 3.184(3) . ?
Pb01 I004 3.210(3) . ?
Pb01 I005 3.122(3) . ?
Pb01 I006 3.278(4) . ?
Pb01 I008 3.135(3) . ?
Pb01 I009 3.150(3) . ?
Pb02 I003 3.186(3) 1_665 ?
Pb02 I004 3.176(3) 1_565 ?
Pb02 I006 3.272(4) 3_676 ?
Pb02 I007 3.116(3) . ?
Pb02 I008 3.149(4) 1_655 ?
Pb02 I009 3.133(3) . ?
I003 Pb02 3.186(3) 1_445 ?
I004 Pb02 3.176(3) 1_545 ?
I006 Pb02 3.272(4) 3_676 ?
I008 Pb02 3.149(4) 1_455 ?
S00B C9 1.90(6) . ?
S00B C32 1.99(6) . ?
N00D H00A 0.8900 . ?
N00D H00B 0.8900 . ?
N00D H00C 0.8900 . ?
N00D C1 1.42(6) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C32 1.44(7) . ?
S40 C9 1.79(6) . ?
S40 C18 1.61(7) . ?
N28 H28A 0.8900 . ?
N28 H28B 0.8900 . ?
N28 H28C 0.8900 . ?
N28 C3 1.41(5) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C18 1.48(7) . ?
C9 C 1.51(6) . ?
C9 C11A 1.61(7) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C4 N1 1.61(6) . ?
N1 H1C 0.8900 . ?
N1 H1D 0.8900 . ?
N1 H1E 0.8900 . ?
C HA 0.9600 . ?
C HB 0.9600 . ?
C HC 0.9600 . ?
C11A H11A 0.9600 . ?
C11A H11B 0.9600 . ?
C11A H11C 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
I003 Pb01 I004 87.75(8) . . ?
I003 Pb01 I006 87.62(9) . . ?
I004 Pb01 I006 87.77(9) . . ?
I005 Pb01 I003 91.88(9) . . ?
I005 Pb01 I004 87.82(9) . . ?
I005 Pb01 I006 175.58(10) . . ?
I005 Pb01 I008 95.20(10) . . ?
I005 Pb01 I009 90.93(9) . . ?
I008 Pb01 I003 93.03(9) . . ?
I008 Pb01 I004 176.85(11) . . ?
I008 Pb01 I006 89.21(9) . . ?
I008 Pb01 I009 90.81(10) . . ?
I009 Pb01 I003 175.01(10) . . ?
I009 Pb01 I004 88.24(9) . . ?
I009 Pb01 I006 89.26(10) . . ?
I003 Pb02 I006 87.27(9) 1_665 3_676 ?
I004 Pb02 I003 88.91(8) 1_565 1_665 ?
I004 Pb02 I006 87.83(9) 1_565 3_676 ?
I007 Pb02 I003 88.13(9) . 1_665 ?
I007 Pb02 I004 91.69(9) . 1_565 ?
I007 Pb02 I006 175.39(10) . 3_676 ?
I007 Pb02 I008 91.18(9) . 1_655 ?
I007 Pb02 I009 95.08(10) . . ?
I008 Pb02 I003 87.60(9) 1_655 1_665 ?
I008 Pb02 I004 175.41(10) 1_655 1_565 ?
I008 Pb02 I006 89.02(10) 1_655 3_676 ?
I009 Pb02 I003 176.57(11) . 1_665 ?
I009 Pb02 I004 92.19(9) . 1_565 ?
I009 Pb02 I006 89.52(9) . 3_676 ?
I009 Pb02 I008 91.12(10) . 1_655 ?
Pb01 I003 Pb02 156.39(11) . 1_445 ?
Pb02 I004 Pb01 155.25(10) 1_545 . ?
Pb02 I006 Pb01 179.29(12) 3_676 . ?
Pb01 I008 Pb02 151.32(12) . 1_455 ?
Pb02 I009 Pb01 151.62(13) . . ?
C9 S00B C32 90(3) . . ?
H00A N00D H00B 109.5 . . ?
H00A N00D H00C 109.5 . . ?
H00B N00D H00C 109.5 . . ?
C1 N00D H00A 109.5 . . ?
C1 N00D H00B 109.5 . . ?
C1 N00D H00C 109.5 . . ?
N00D C1 H1A 107.7 . . ?
N00D C1 H1B 107.7 . . ?
N00D C1 C32 119(4) . . ?
H1A C1 H1B 107.1 . . ?
C32 C1 H1A 107.7 . . ?
C32 C1 H1B 107.7 . . ?
C18 S40 C9 116(3) . . ?
H28A N28 H28B 109.5 . . ?
H28A N28 H28C 109.5 . . ?
H28B N28 H28C 109.5 . . ?
C3 N28 H28A 109.5 . . ?
C3 N28 H28B 109.5 . . ?
C3 N28 H28C 109.5 . . ?
N28 C3 H3A 109.4 . . ?
N28 C3 H3B 109.4 . . ?
N28 C3 C18 111(4) . . ?
H3A C3 H3B 108.0 . . ?
C18 C3 H3A 109.4 . . ?
C18 C3 H3B 109.4 . . ?
S40 C9 S00B 110(3) . . ?
C C9 S00B 102(3) . . ?
C C9 S40 102(3) . . ?
C C9 C11A 114(4) . . ?
C11A C9 S00B 117(3) . . ?
C11A C9 S40 111(3) . . ?
S00B C32 H32A 110.7 . . ?
S00B C32 H32B 110.7 . . ?
C1 C32 S00B 105(4) . . ?
C1 C32 H32A 110.7 . . ?
C1 C32 H32B 110.7 . . ?
H32A C32 H32B 108.8 . . ?
S40 C18 H18A 107.1 . . ?
S40 C18 H18B 107.1 . . ?
C3 C18 S40 121(4) . . ?
C3 C18 H18A 107.1 . . ?
C3 C18 H18B 107.1 . . ?
H18A C18 H18B 106.8 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
N1 C4 H4C 109.5 . . ?
C4 N1 H1C 109.5 . . ?
C4 N1 H1D 109.5 . . ?
C4 N1 H1E 109.5 . . ?
H1C N1 H1D 109.5 . . ?
H1C N1 H1E 109.5 . . ?
H1D N1 H1E 109.5 . . ?
C9 C HA 109.5 . . ?
C9 C HB 109.5 . . ?
C9 C HC 109.5 . . ?
HA C HB 109.5 . . ?
HA C HC 109.5 . . ?
HB C HC 109.5 . . ?
C9 C11A H11A 109.5 . . ?
C9 C11A H11B 109.5 . . ?
C9 C11A H11C 109.5 . . ?
H11A C11A H11B 109.5 . . ?
H11A C11A H11C 109.5 . . ?
H11B C11A H11C 109.5 . . ?

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
N00D C1 C32 S00B -58(5) . . . . ?
N28 C3 C18 S40 -56(6) . . . . ?
C9 S40 C18 C3 -93(5) . . . . ?
C32 S00B C9 S40 -76(3) . . . . ?
C32 S00B C9 C 177(3) . . . . ?
C32 S00B C9 C11A 52(4) . . . . ?
C18 S40 C9 S00B -58(4) . . . . ?
C18 S40 C9 C 50(4) . . . . ?
C18 S40 C9 C11A 171(4) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.351
_oxdiff_exptl_absorpt_empirical_full_min 0.452
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.96108
2 0.03892

####################################################################### 
# 
# 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_(MSBA)(MA)2Pb3I10
_database_code_depnum_ccdc_archive 'CCDC 2249141'
loop_
_audit_author_name
_audit_author_address
'Wenxuan Li'
;Sun Yat sen University
China
;
_audit_update_record             
;
2023-03-16 deposited with the CCDC.	2023-10-02 downloaded from the CCDC.
;
_audit_creation_date             2022-11-12
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'I10 Pb3, C5 H16 N2 S2, 2(C H6 N)'
_chemical_formula_sum            'C7 H28 I10 N4 Pb3 S2'
_chemical_formula_weight         2123.02
_chemical_melting_point          ?
_chemical_oxdiff_formula         CHNSPbI
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           15
_space_group_name_H-M_alt        'I 1 2/a 1'
_space_group_name_Hall           '-I 2ya'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   8.7507(2)
_cell_length_b                   8.80529(19)
_cell_length_c                   49.5412(13)
_cell_angle_alpha                90
_cell_angle_beta                 93.213(2)
_cell_angle_gamma                90
_cell_volume                     3811.26(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    10408
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.6040
_cell_measurement_theta_min      2.3370
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    21.435
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.26629
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.120a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    3.700
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             3624
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0599
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.868
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       66
_diffrn_reflns_limit_l_min       -69
_diffrn_reflns_number            27216
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.868
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.586
_diffrn_reflns_theta_min         2.344
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.868
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -9.00  16.00   0.50    3.50    --   -7.87 -99.00 -30.00   50
  2  ω    -18.00  44.00   0.50    3.50    --    7.17 -99.00  60.00  124
  3  ω    -16.00  10.00   0.50    3.50    --    7.17 -99.00 150.00   52
  4  ω    -70.00 -12.00   0.50    3.50    --   -7.87 -38.00 120.00  116
  5  ω    -79.00  -1.00   0.50    3.50    --   -7.87 -57.00  60.00  156
  6  ω    -77.00 -44.00   0.50    5.00    --   -7.87 159.00  69.00   66
  7  ω    -15.00  41.00   0.50    5.00    --    7.17 -99.00 -60.00  112
  8  ω    -59.00  17.00   0.50    5.00    --    7.17 -57.00 -30.00  152
  9  ω    -16.00  17.00   0.50    5.00    --   -7.87 -99.00 -30.00   66
 10  ω    -78.00 -53.00   0.50    5.00    --   -7.87 -38.00-180.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0028712500
_diffrn_orient_matrix_UB_12      0.0644005500
_diffrn_orient_matrix_UB_13      -0.0085605500
_diffrn_orient_matrix_UB_21      0.0073399000
_diffrn_orient_matrix_UB_22      -0.0483575000
_diffrn_orient_matrix_UB_23      -0.0113044000
_diffrn_orient_matrix_UB_31      -0.0807874000
_diffrn_orient_matrix_UB_32      -0.0021272000
_diffrn_orient_matrix_UB_33      -0.0021351000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4438
_reflns_number_total             5014
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_refine_diff_density_max         2.677
_refine_diff_density_min         -3.508
_refine_diff_density_rms         0.469
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.218
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     124
_refine_ls_number_reflns         5014
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0664
_refine_ls_R_factor_gt           0.0572
_refine_ls_restrained_S_all      1.218
_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)+531.0102P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1211
_refine_ls_wR_factor_ref         0.1238
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.919(2)
 0.081(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Others
 Fixed Sof: H13A(0.5) H13B(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C10(H10A,H10B), C13(H13A,H13B)
4.b Idealised Me refined as rotating group:
 N12(H12A,H12B,H12C), N14(H14A,H14B,H14C), C15(H15A,H15B,H15C)
;
_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 0.80212(6) 0.24825(6) 0.38133(2) 0.01130(12) Uani 1 1 d . . . . .
Pb2 Pb 0.7500 0.2500 0.2500 0.01168(15) Uani 1 2 d S . P . .
I3 I 1.06224(11) 0.06208(10) 0.24953(2) 0.0178(2) Uani 1 1 d . . . . .
I4 I 0.59654(11) 0.54432(10) 0.37565(2) 0.0176(2) Uani 1 1 d . . . . .
I5 I 0.78109(11) 0.25543(11) 0.31398(2) 0.01627(19) Uani 1 1 d . . . . .
I6 I 0.80424(12) 0.28580(11) 0.44301(2) 0.0198(2) Uani 1 1 d . . . . .
I7 I 0.51129(12) 0.04153(11) 0.38142(2) 0.0228(2) Uani 1 1 d . . . . .
S9 S 0.4084(6) 0.2781(12) 0.48982(12) 0.073(3) Uani 1 1 d . . . . .
N12 N 0.3804(15) 0.3209(15) 0.4274(3) 0.021(3) Uani 1 1 d . . . . .
H12A H 0.3424 0.3536 0.4109 0.025 Uiso 1 1 calc R U . . .
H12B H 0.4665 0.2651 0.4253 0.025 Uiso 1 1 calc R U . . .
H12C H 0.4034 0.4024 0.4381 0.025 Uiso 1 1 calc R U . . .
N14 N 0.1864(17) 0.3335(17) 0.3047(3) 0.028(3) Uani 1 1 d . . . . .
H14A H 0.2061 0.3401 0.2869 0.033 Uiso 1 1 calc R U . . .
H14B H 0.1987 0.4265 0.3125 0.033 Uiso 1 1 calc R U . . .
H14C H 0.0885 0.3013 0.3062 0.033 Uiso 1 1 calc R U . . .
C15 C 0.296(3) 0.222(2) 0.3186(5) 0.044(6) Uani 1 1 d . . . . .
H15A H 0.3235 0.1435 0.3057 0.066 Uiso 1 1 calc R U . . .
H15B H 0.2465 0.1740 0.3337 0.066 Uiso 1 1 calc R U . . .
H15C H 0.3883 0.2753 0.3254 0.066 Uiso 1 1 calc R U . . .
C11 C 0.265(2) 0.227(3) 0.4399(4) 0.047(6) Uani 1 1 d . . . . .
H11A H 0.2285 0.1475 0.4269 0.057 Uiso 1 1 calc R U . . .
H11B H 0.1769 0.2906 0.4441 0.057 Uiso 1 1 calc R U . . .
C10 C 0.329(4) 0.152(2) 0.4651(4) 0.056(7) Uani 1 1 d . . . . .
H10A H 0.4085 0.0791 0.4604 0.067 Uiso 1 1 calc R U . . .
H10B H 0.2457 0.0941 0.4732 0.067 Uiso 1 1 calc R U . . .
C13 C 0.2500 0.379(4) 0.5000 0.072(14) Uani 1 2 d S T P . .
H13A H 0.2853 0.4458 0.5152 0.086 Uiso 0.5 1 calc R U P . .
H13B H 0.2147 0.4459 0.4848 0.086 Uiso 0.5 1 calc R U P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 I4 3.1709(10) . ?
Pb1 I4 3.1834(10) 6_665 ?
Pb1 I5 3.3320(10) . ?
Pb1 I6 3.0727(11) . ?
Pb1 I7 3.1401(11) 6_655 ?
Pb1 I7 3.1291(11) . ?
Pb2 I3 3.1955(9) . ?
Pb2 I3 3.2011(9) 6 ?
Pb2 I3 3.1955(9) 7_655 ?
Pb2 I3 3.2011(9) 4_655 ?
Pb2 I5 3.1663(9) 7_655 ?
Pb2 I5 3.1663(9) . ?
I3 Pb2 3.2011(9) 4_645 ?
I4 Pb1 3.1834(10) 6_565 ?
I7 Pb1 3.1401(11) 6 ?
S9 C10 1.76(2) . ?
S9 C13 1.745(17) . ?
N12 H12A 0.9100 . ?
N12 H12B 0.9100 . ?
N12 H12C 0.9100 . ?
N12 C11 1.47(2) . ?
N14 H14A 0.9100 . ?
N14 H14B 0.9100 . ?
N14 H14C 0.9100 . ?
N14 C15 1.51(2) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C10 1.49(3) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C13 S9 1.745(17) 2_556 ?
C13 H13A 0.9900 . ?
C13 H13B 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
I4 Pb1 I4 88.763(14) . 6_665 ?
I4 Pb1 I5 84.27(3) 6_665 . ?
I4 Pb1 I5 84.05(3) . . ?
I6 Pb1 I4 88.37(3) . . ?
I6 Pb1 I4 93.80(3) . 6_665 ?
I6 Pb1 I5 172.21(3) . . ?
I6 Pb1 I7 91.19(3) . . ?
I6 Pb1 I7 96.60(3) . 6_655 ?
I7 Pb1 I4 175.00(3) . 6_665 ?
I7 Pb1 I4 89.53(3) 6_655 6_665 ?
I7 Pb1 I4 91.20(3) . . ?
I7 Pb1 I4 174.84(3) 6_655 . ?
I7 Pb1 I5 90.93(3) 6_655 . ?
I7 Pb1 I5 90.75(3) . . ?
I7 Pb1 I7 90.078(14) . 6_655 ?
I3 Pb2 I3 180.0 . 7_655 ?
I3 Pb2 I3 89.665(8) . 6 ?
I3 Pb2 I3 90.335(8) . 4_655 ?
I3 Pb2 I3 89.666(8) 7_655 4_655 ?
I3 Pb2 I3 180.0 4_655 6 ?
I3 Pb2 I3 90.334(8) 7_655 6 ?
I5 Pb2 I3 87.96(3) 7_655 6 ?
I5 Pb2 I3 89.41(3) 7_655 7_655 ?
I5 Pb2 I3 89.41(3) . . ?
I5 Pb2 I3 90.59(3) 7_655 . ?
I5 Pb2 I3 92.04(3) 7_655 4_655 ?
I5 Pb2 I3 90.59(3) . 7_655 ?
I5 Pb2 I3 92.04(3) . 6 ?
I5 Pb2 I3 87.96(3) . 4_655 ?
I5 Pb2 I5 180.00(3) . 7_655 ?
Pb2 I3 Pb2 152.03(3) . 4_645 ?
Pb1 I4 Pb1 157.19(4) . 6_565 ?
Pb2 I5 Pb1 177.37(4) . . ?
Pb1 I7 Pb1 161.22(4) . 6 ?
C13 S9 C10 103.3(12) . . ?
H12A N12 H12B 109.5 . . ?
H12A N12 H12C 109.5 . . ?
H12B N12 H12C 109.5 . . ?
C11 N12 H12A 109.5 . . ?
C11 N12 H12B 109.5 . . ?
C11 N12 H12C 109.5 . . ?
H14A N14 H14B 109.5 . . ?
H14A N14 H14C 109.5 . . ?
H14B N14 H14C 109.5 . . ?
C15 N14 H14A 109.5 . . ?
C15 N14 H14B 109.5 . . ?
C15 N14 H14C 109.5 . . ?
N14 C15 H15A 109.5 . . ?
N14 C15 H15B 109.5 . . ?
N14 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N12 C11 H11A 109.3 . . ?
N12 C11 H11B 109.3 . . ?
N12 C11 C10 111.8(18) . . ?
H11A C11 H11B 107.9 . . ?
C10 C11 H11A 109.3 . . ?
C10 C11 H11B 109.3 . . ?
S9 C10 H10A 108.5 . . ?
S9 C10 H10B 108.5 . . ?
C11 C10 S9 114.9(16) . . ?
C11 C10 H10A 108.5 . . ?
C11 C10 H10B 108.5 . . ?
H10A C10 H10B 107.5 . . ?
S9 C13 S9 118.7(19) 2_556 . ?
S9 C13 H13A 107.6 2_556 . ?
S9 C13 H13A 107.6 . . ?
S9 C13 H13B 107.6 2_556 . ?
S9 C13 H13B 107.6 . . ?
H13A C13 H13B 107.1 . . ?

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
N12 C11 C10 S9 56(3) . . . . ?
C10 S9 C13 S9 52.5(8) . . . 2_556 ?
C13 S9 C10 C11 67(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 6.727
_oxdiff_exptl_absorpt_empirical_full_min 0.350
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.919(2)
2 0.081(2)

####################################################################### 
# 
# 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_(PDSBA)(MA)2Pb3I10
_database_code_depnum_ccdc_archive 'CCDC 2249143'
loop_
_audit_author_name
_audit_author_address
'Wenxuan Li'
;Sun Yat sen University
China
;
_audit_update_record             
;
2023-03-16 deposited with the CCDC.	2023-10-02 downloaded from the CCDC.
;
_audit_creation_date             2022-11-12
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'I10 Pb3, 2(C H6 N), C7 H20 N2 S2'
_chemical_formula_sum            'C9 H32 I10 N4 Pb3 S2'
_chemical_formula_weight         2151.07
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         CHNSPbI
_chemical_oxdiff_usercomment     CHNSPbI
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           7
_space_group_name_H-M_alt        'P 1 c 1'
_space_group_name_Hall           'P -2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'

_cell_length_a                   26.1723(6)
_cell_length_b                   8.7520(2)
_cell_length_c                   8.7431(2)
_cell_angle_alpha                90
_cell_angle_beta                 91.710(2)
_cell_angle_gamma                90
_cell_volume                     2001.80(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    22733
_cell_measurement_temperature    99.9(2)
_cell_measurement_theta_max      30.7010
_cell_measurement_theta_min      2.3200
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    20.408
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.32703
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.60a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear pale yellow'
_exptl_crystal_density_diffrn    3.569
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1844
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0648
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            37435
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.327
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -31.00  53.00   0.50   10.00    --   -7.94  71.00  -7.00  168
  2  ω    -80.00  -1.00   0.50   10.00    --   -7.94 -71.00-138.00  158
  3  ω      4.00  35.00   0.50   10.00    --    7.16 -99.00  90.00   62
  4  ω    -17.00   8.00   0.50   10.00    --   -7.94 -99.00 -90.00   50
  5  ω    -18.00  17.00   0.50   10.00    --   -7.94 -99.00  60.00   70
  6  ω    -11.00  15.00   0.50   10.00    --   -7.94 -71.00-138.00   52
  7  ω    -17.00  44.00   0.50   10.00    --    7.16 -99.00  30.00  122
  8  ω     36.00  64.00   0.50   10.00    --   -7.94  57.00-120.00   56
  9  ω    -77.00 -12.00   0.50   10.00    --   -7.94 -38.00  90.00  130
 10  ω    -24.00   1.00   0.50   10.00    --   -7.94  57.00-120.00   50
 11  ω    -17.00   9.00   0.50   10.00    --   -7.94 -99.00-180.00   52
 12  ω    -18.00   7.00   0.50   10.00    --   -7.94 -99.00  30.00   50
 13  ω    -56.00 -31.00   0.50   10.00    --   -7.94 -71.00-138.00   50
 14  ω    -41.00 -16.00   0.50   10.00    --    7.16 -71.00-138.00   50
 15  ω      7.00  32.00   0.50   10.00    --    7.16  77.00-180.00   50
 16  ω    -14.00  20.00   0.50   10.00    --    7.16  19.00 120.00   68
 17  ω    -25.00  70.00   0.50   10.00    --   -7.94  19.00-180.00  190
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0253902000
_diffrn_orient_matrix_UB_12      -0.0185855000
_diffrn_orient_matrix_UB_13      0.0191198000
_diffrn_orient_matrix_UB_21      -0.0001168000
_diffrn_orient_matrix_UB_22      0.0617144000
_diffrn_orient_matrix_UB_23      0.0525923000
_diffrn_orient_matrix_UB_31      -0.0094990000
_diffrn_orient_matrix_UB_32      0.0490910000
_diffrn_orient_matrix_UB_33      -0.0588387000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.976
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.943
_reflns_number_gt                7295
_reflns_number_total             7539
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.60a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.60a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.60a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_refine_diff_density_max         6.108
_refine_diff_density_min         -4.497
_refine_diff_density_rms         0.698
_refine_ls_abs_structure_details 
;
 Flack x determined using 3204 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.382(6)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         7539
_refine_ls_number_restraints     44
_refine_ls_R_factor_all          0.0714
_refine_ls_R_factor_gt           0.0697
_refine_ls_restrained_S_all      1.144
_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)+(0.0626P)²+247.0105P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1776
_refine_ls_wR_factor_ref         0.1785
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.9596(16)
 0.0404(16)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C30) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C70)
\\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms
of 0.02
Uanis(C30) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(I009) \\sim Ueq, Uanis(C1)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4.a Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C43(H43A,H43B), C1(H1A,H1B), C51(H51A,H51B)
4.b Idealised Me refined as rotating group:
 N21(H21A,H21B,H21C), C22(H22A,H22B,H22C), N2(H2A,H2B,H2C), C19(H19A,H19B,
 H19C), C49(H49A,H49B,H49C), N16(H16A,H16B,H16C), N38(H38A,H38B,H38C), C70(H70A,
 H70B,H70C)
;
_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
Pb01 Pb -0.60790(6) 0.74416(17) 0.10410(14) 0.0075(4) Uani 1 1 d . . . . .
Pb00 Pb -0.35989(9) 0.75884(19) 0.1330(2) 0.0079(3) Uani 1 1 d . . . . .
I003 I -0.60648(13) 0.9479(3) 0.4047(4) 0.0117(6) Uani 1 1 d . . . . .
I005 I -0.72621(12) 0.7542(3) 0.0874(4) 0.0151(7) Uani 1 1 d . . . . .
I006 I -0.60334(14) 0.4355(3) 0.2893(4) 0.0188(7) Uani 1 1 d . . . . .
I007 I -0.48197(15) 0.7473(3) 0.1109(4) 0.0138(7) Uani 1 1 d . . . . .
I008 I -0.23937(15) 0.7478(3) 0.1315(5) 0.0153(7) Uani 1 1 d . . . . .
I009 I -0.36043(15) 1.0701(3) 0.3108(4) 0.0155(6) Uani 1 1 d . U . . .
I00A I -0.35878(13) 0.5549(3) 0.4364(4) 0.0127(6) Uiso 1 1 d . . . . .
Pb1 Pb -0.11189(6) 0.75257(18) 0.14267(17) 0.0086(4) Uani 1 1 d . . . . .
I3 I 0.00483(12) 0.7167(4) 0.1701(4) 0.0164(6) Uani 1 1 d . . . . .
I5 I -0.12278(13) 0.5428(4) -0.1509(4) 0.0171(7) Uani 1 1 d . . . . .
I6 I -0.11061(14) 1.0402(4) -0.0669(4) 0.0200(7) Uani 1 1 d . . . . .
N21 N -0.2570(18) 0.664(5) -0.280(6) 0.037(11) Uani 1 1 d . . . . .
H21A H -0.2896 0.6448 -0.3141 0.044 Uiso 1 1 calc R U . . .
H21B H -0.2573 0.7034 -0.1843 0.044 Uiso 1 1 calc R U . . .
H21C H -0.2389 0.5750 -0.2791 0.044 Uiso 1 1 calc R U . . .
C22 C -0.2320(18) 0.778(6) -0.388(6) 0.019(10) Uani 1 1 d . U . . .
H22A H -0.2490 0.7733 -0.4897 0.029 Uiso 1 1 calc R U . . .
H22B H -0.1957 0.7533 -0.3974 0.029 Uiso 1 1 calc R U . . .
H22C H -0.2353 0.8820 -0.3471 0.029 Uiso 1 1 calc R U . . .
S1 S 0.1825(5) 0.8739(14) 0.6924(15) 0.023(3) Uani 1 1 d . . . . .
N2 N 0.2989(16) 0.834(5) 0.677(5) 0.022(9) Uani 1 1 d . . . . .
H2A H 0.3114 0.9226 0.6380 0.027 Uiso 1 1 calc R U . . .
H2B H 0.3253 0.7737 0.7096 0.027 Uiso 1 1 calc R U . . .
H2C H 0.2788 0.8564 0.7574 0.027 Uiso 1 1 calc R U . . .
C27 C 0.268(2) 0.753(6) 0.556(7) 0.029(12) Uani 1 1 d . U . . .
H27A H 0.2871 0.7520 0.4601 0.035 Uiso 1 1 calc R U . . .
H27B H 0.2631 0.6454 0.5879 0.035 Uiso 1 1 calc R U . . .
C30 C 0.1415(17) 0.711(5) 0.731(5) 0.016(9) Uani 1 1 d . U . . .
C43 C 0.218(2) 0.820(6) 0.525(6) 0.031(12) Uani 1 1 d . U . . .
H43A H 0.1976 0.7470 0.4635 0.037 Uiso 1 1 calc R U . . .
H43B H 0.2231 0.9125 0.4617 0.037 Uiso 1 1 calc R U . . .
S2 S 0.0946(5) 0.6824(15) 0.5707(15) 0.024(3) Uani 1 1 d . . . . .
C19 C 0.118(2) 0.739(7) 0.885(7) 0.040(15) Uani 1 1 d . . . . .
H19A H 0.1455 0.7341 0.9655 0.060 Uiso 1 1 calc R U . . .
H19B H 0.0928 0.6600 0.9045 0.060 Uiso 1 1 calc R U . . .
H19C H 0.1023 0.8396 0.8861 0.060 Uiso 1 1 calc R U . . .
C1 C 0.004(2) 0.818(6) 0.679(6) 0.028(11) Uani 1 1 d . U . . .
H1A H 0.0128 0.7954 0.7874 0.033 Uiso 1 1 calc R U . . .
H1B H -0.0183 0.9100 0.6754 0.033 Uiso 1 1 calc R U . . .
C49 C 0.1705(17) 0.553(6) 0.742(6) 0.025(11) Uani 1 1 d . . . . .
H49A H 0.2071 0.5717 0.7600 0.038 Uiso 1 1 calc R U . . .
H49B H 0.1654 0.4975 0.6452 0.038 Uiso 1 1 calc R U . . .
H49C H 0.1572 0.4928 0.8258 0.038 Uiso 1 1 calc R U . . .
C51 C 0.052(2) 0.848(6) 0.592(5) 0.024(11) Uani 1 1 d . . . . .
H51A H 0.0715 0.9303 0.6448 0.029 Uiso 1 1 calc R U . . .
H51B H 0.0420 0.8856 0.4887 0.029 Uiso 1 1 calc R U . . .
N16 N -0.0223(17) 0.691(4) 0.609(5) 0.019(9) Uani 1 1 d . . . . .
H16A H -0.0392 0.7221 0.5224 0.023 Uiso 1 1 calc R U . . .
H16B H -0.0451 0.6520 0.6757 0.023 Uiso 1 1 calc R U . . .
H16C H 0.0007 0.6172 0.5857 0.023 Uiso 1 1 calc R U . . .
N38 N -0.464(2) 0.661(6) 0.707(5) 0.047(14) Uani 1 1 d . . . . .
H38A H -0.4313 0.6339 0.6826 0.056 Uiso 1 1 calc R U . . .
H38B H -0.4834 0.5757 0.7127 0.056 Uiso 1 1 calc R U . . .
H38C H -0.4630 0.7104 0.7982 0.056 Uiso 1 1 calc R U . . .
C70 C -0.485(3) 0.760(8) 0.591(8) 0.047(17) Uani 1 1 d . U . . .
H70A H -0.4590 0.7776 0.5130 0.071 Uiso 1 1 calc R U . . .
H70B H -0.4941 0.8574 0.6368 0.071 Uiso 1 1 calc R U . . .
H70C H -0.5149 0.7121 0.5428 0.071 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
Pb01 I003 3.176(3) . ?
Pb01 I003 3.210(3) 2_574 ?
Pb01 I005 3.097(3) . ?
Pb01 I006 3.150(3) . ?
Pb01 I006 3.175(4) 2_564 ?
Pb01 I007 3.295(4) . ?
Pb00 I007 3.197(4) . ?
Pb00 I008 3.156(4) . ?
Pb00 I009 3.137(3) . ?
Pb00 I009 3.190(4) 2_574 ?
Pb00 I00A 3.240(3) 2_564 ?
Pb00 I00A 3.197(4) . ?
I003 Pb01 3.210(3) 2_575 ?
I006 Pb01 3.175(4) 2_565 ?
I008 Pb1 3.335(4) . ?
I009 Pb00 3.190(4) 2_575 ?
I00A Pb00 3.240(3) 2_565 ?
Pb1 I3 3.073(3) . ?
Pb1 I5 3.162(4) . ?
Pb1 I5 3.171(3) 2_565 ?
Pb1 I6 3.115(4) . ?
Pb1 I6 3.120(3) 2_575 ?
I5 Pb1 3.171(3) 2_564 ?
I6 Pb1 3.120(3) 2_574 ?
N21 H21A 0.9100 . ?
N21 H21B 0.9100 . ?
N21 H21C 0.9100 . ?
N21 C22 1.54(6) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
S1 C30 1.82(5) . ?
S1 C43 1.82(5) . ?
N2 H2A 0.9100 . ?
N2 H2B 0.9100 . ?
N2 H2C 0.9100 . ?
N2 C27 1.50(7) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C43 1.44(8) . ?
C30 S2 1.85(5) . ?
C30 C19 1.51(7) . ?
C30 C49 1.58(7) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
S2 C51 1.84(6) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C51 1.51(7) . ?
C1 N16 1.44(7) . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
N16 H16A 0.9100 . ?
N16 H16B 0.9100 . ?
N16 H16C 0.9100 . ?
N38 H38A 0.9100 . ?
N38 H38B 0.9100 . ?
N38 H38C 0.9100 . ?
N38 C70 1.43(8) . ?
C70 H70A 0.9800 . ?
C70 H70B 0.9800 . ?
C70 H70C 0.9800 . ?

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
I003 Pb01 I003 88.74(4) . 2_574 ?
I003 Pb01 I007 89.62(10) . . ?
I003 Pb01 I007 88.57(9) 2_574 . ?
I005 Pb01 I003 90.58(9) . . ?
I005 Pb01 I003 88.76(9) . 2_574 ?
I005 Pb01 I006 92.09(10) . 2_564 ?
I005 Pb01 I006 94.07(10) . . ?
I005 Pb01 I007 177.32(10) . . ?
I006 Pb01 I003 174.72(10) 2_564 . ?
I006 Pb01 I003 176.52(12) . 2_574 ?
I006 Pb01 I003 93.25(10) . . ?
I006 Pb01 I003 86.78(9) 2_564 2_574 ?
I006 Pb01 I006 91.10(5) . 2_564 ?
I006 Pb01 I007 87.50(10) 2_564 . ?
I006 Pb01 I007 88.59(10) . . ?
I007 Pb00 I00A 88.04(10) . 2_564 ?
I008 Pb00 I007 174.86(12) . . ?
I008 Pb00 I009 89.37(11) . 2_574 ?
I008 Pb00 I00A 90.11(10) . . ?
I008 Pb00 I00A 86.97(10) . 2_564 ?
I009 Pb00 I007 89.05(11) 2_574 . ?
I009 Pb00 I007 92.18(11) . . ?
I009 Pb00 I008 92.75(10) . . ?
I009 Pb00 I009 91.73(5) . 2_574 ?
I009 Pb00 I00A 177.65(13) . 2_564 ?
I009 Pb00 I00A 85.94(10) 2_574 2_564 ?
I009 Pb00 I00A 174.05(11) 2_574 . ?
I009 Pb00 I00A 94.22(11) . . ?
I00A Pb00 I007 90.96(10) . . ?
I00A Pb00 I00A 88.11(5) . 2_564 ?
Pb01 I003 Pb01 157.05(11) . 2_575 ?
Pb01 I006 Pb01 150.30(13) . 2_565 ?
Pb00 I007 Pb01 177.23(13) . . ?
Pb00 I008 Pb1 176.88(12) . . ?
Pb00 I009 Pb00 147.72(12) . 2_575 ?
Pb00 I00A Pb00 155.98(12) . 2_565 ?
I3 Pb1 I008 172.84(9) . . ?
I3 Pb1 I5 93.98(10) . . ?
I3 Pb1 I5 88.76(10) . 2_565 ?
I3 Pb1 I6 95.75(11) . . ?
I3 Pb1 I6 90.54(10) . 2_575 ?
I5 Pb1 I008 84.23(9) 2_565 . ?
I5 Pb1 I008 84.44(10) . . ?
I5 Pb1 I5 88.93(5) . 2_565 ?
I6 Pb1 I008 91.22(10) . . ?
I6 Pb1 I008 91.00(10) 2_575 . ?
I6 Pb1 I5 89.65(10) . . ?
I6 Pb1 I5 175.44(12) 2_575 . ?
I6 Pb1 I5 175.35(12) . 2_565 ?
I6 Pb1 I5 90.55(10) 2_575 2_565 ?
I6 Pb1 I6 90.51(4) . 2_575 ?
Pb1 I5 Pb1 158.13(14) . 2_564 ?
Pb1 I6 Pb1 161.56(13) . 2_574 ?
H21A N21 H21B 109.5 . . ?
H21A N21 H21C 109.5 . . ?
H21B N21 H21C 109.5 . . ?
C22 N21 H21A 109.5 . . ?
C22 N21 H21B 109.5 . . ?
C22 N21 H21C 109.5 . . ?
N21 C22 H22A 109.5 . . ?
N21 C22 H22B 109.5 . . ?
N21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C30 S1 C43 106(2) . . ?
H2A N2 H2B 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
C27 N2 H2A 109.5 . . ?
C27 N2 H2B 109.5 . . ?
C27 N2 H2C 109.5 . . ?
N2 C27 H27A 108.8 . . ?
N2 C27 H27B 108.8 . . ?
H27A C27 H27B 107.7 . . ?
C43 C27 N2 114(5) . . ?
C43 C27 H27A 108.8 . . ?
C43 C27 H27B 108.8 . . ?
S1 C30 S2 110(2) . . ?
C19 C30 S1 107(4) . . ?
C19 C30 S2 115(4) . . ?
C19 C30 C49 107(4) . . ?
C49 C30 S1 114(3) . . ?
C49 C30 S2 103(3) . . ?
S1 C43 H43A 108.3 . . ?
S1 C43 H43B 108.3 . . ?
C27 C43 S1 116(4) . . ?
C27 C43 H43A 108.3 . . ?
C27 C43 H43B 108.3 . . ?
H43A C43 H43B 107.4 . . ?
C51 S2 C30 102(2) . . ?
C30 C19 H19A 109.5 . . ?
C30 C19 H19B 109.5 . . ?
C30 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
H1A C1 H1B 108.4 . . ?
C51 C1 H1A 110.0 . . ?
C51 C1 H1B 110.0 . . ?
N16 C1 H1A 110.0 . . ?
N16 C1 H1B 110.0 . . ?
N16 C1 C51 108(4) . . ?
C30 C49 H49A 109.5 . . ?
C30 C49 H49B 109.5 . . ?
C30 C49 H49C 109.5 . . ?
H49A C49 H49B 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
S2 C51 H51A 108.4 . . ?
S2 C51 H51B 108.4 . . ?
C1 C51 S2 116(4) . . ?
C1 C51 H51A 108.4 . . ?
C1 C51 H51B 108.4 . . ?
H51A C51 H51B 107.4 . . ?
C1 N16 H16A 109.5 . . ?
C1 N16 H16B 109.5 . . ?
C1 N16 H16C 109.5 . . ?
H16A N16 H16B 109.5 . . ?
H16A N16 H16C 109.5 . . ?
H16B N16 H16C 109.5 . . ?
H38A N38 H38B 109.5 . . ?
H38A N38 H38C 109.5 . . ?
H38B N38 H38C 109.5 . . ?
C70 N38 H38A 109.5 . . ?
C70 N38 H38B 109.5 . . ?
C70 N38 H38C 109.5 . . ?
N38 C70 H70A 109.5 . . ?
N38 C70 H70B 109.5 . . ?
N38 C70 H70C 109.5 . . ?
H70A C70 H70B 109.5 . . ?
H70A C70 H70C 109.5 . . ?
H70B C70 H70C 109.5 . . ?

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 C30 S2 C51 -71(3) . . . . ?
N2 C27 C43 S1 -45(6) . . . . ?
C30 S1 C43 C27 -94(4) . . . . ?
C30 S2 C51 C1 -96(4) . . . . ?
C43 S1 C30 S2 -64(3) . . . . ?
C43 S1 C30 C19 170(4) . . . . ?
C43 S1 C30 C49 51(4) . . . . ?
C19 C30 S2 C51 51(4) . . . . ?
C49 C30 S2 C51 167(3) . . . . ?
N16 C1 C51 S2 -54(5) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.008
_oxdiff_exptl_absorpt_empirical_full_min 0.469
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.9596(16)
2 0.0404(16)

