# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 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_n=1_(DicI)PbI4
_database_code_depnum_ccdc_archive 'CCDC 2283257'
loop_
_audit_author_name
_audit_author_address
'Nicolas Mercier'
;UNIV Angers, UMR CNRS
France
;
_audit_update_record             
;
2023-11-24 deposited with the CCDC.	2023-11-30 downloaded from the CCDC.
;
#=======================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic        
; ?
;
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_iupac          ?
_chemical_formula_sum            'C3 H11 I5 N2 Pb1'
_chemical_formula_weight         916.8
_chemical_melting_point          ?
_chemical_compound_source        ?
_chemical_absolute_configuration .

#=======================================================================

# 6. CRYSTAL DATA

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'C m c e'
_symmetry_space_group_name_Hall  '-C -2x;-2ybc;-2zbc'
_symmetry_Int_Tables_number      64

loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,-y+1/2,z+1/2
3 -x,y+1/2,-z+1/2
4 x,-y,-z
5 -x,-y,-z
6 x,y+1/2,-z+1/2
7 x,-y+1/2,z+1/2
8 -x,y,z
9 x+1/2,y+1/2,z
10 -x+1/2,-y,z+1/2
11 -x+1/2,y,-z+1/2
12 x+1/2,-y+1/2,-z
13 -x+1/2,-y+1/2,-z
14 x+1/2,y,-z+1/2
15 x+1/2,-y,z+1/2
16 -x+1/2,y+1/2,z

_cell_length_a                   20.1168(15)
_cell_length_b                   12.6758(10)
_cell_length_c                   12.2263(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3117.7(4)


_cell_formula_units_Z            8

_cell_measurement_reflns_used    2509
_cell_measurement_theta_min      4.41
_cell_measurement_theta_max      70.6
_cell_measurement_temperature    294.2(8)
_cell_special_details            
; ?
;

_exptl_crystal_density_diffrn    3.9067
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             3120

_exptl_absorpt_coefficient_mu    98.516
_exptl_crystal_description       'plate-like crystals'
_exptl_crystal_size_max          0.081
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.016
_exptl_crystal_size_rad          ?
_exptl_crystal_colour            red
_exptl_absorpt_correction_type   multi-scan
_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_absorpt_correction_T_min  0.083
_exptl_absorpt_correction_T_max  1
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
? ? ? ?

#=======================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           ?


_diffrn_ambient_temperature      294.2
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_power             ?
_diffrn_source_voltage           ?
_diffrn_source_current           ?
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'SuperNova, Single source at offset/far, AtlasS2'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1990
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support ?


_diffrn_reflns_number            10141
_diffrn_reflns_theta_min         4.4
_diffrn_reflns_theta_max         71.54
_diffrn_reflns_theta_full        71.54
_diffrn_measured_fraction_theta_max 1
_diffrn_measured_fraction_theta_full 1
_diffrn_reflns_av_R_equivalents  0.0916
_diffrn_reflns_av_unetI/netI     0.0431
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_reduction_process ?

_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?

_diffrn_radiation_probe          X-ray

#=======================================================================

# 8. REFINEMENT DATA

_refine_special_details          
; ?
;

_reflns_number_total             1462
_reflns_number_gt                1147
_reflns_threshold_expression     I>2σ(I)

_refine_ls_structure_factor_coef F
_refine_ls_R_factor_gt           0.0502
_refine_ls_wR_factor_gt          0.0533
_refine_ls_R_factor_all          0.0656
_refine_ls_wR_factor_ref         0.0551
_refine_ls_goodness_of_fit_ref   1.56
_refine_ls_goodness_of_fit_gt    1.71
_refine_ls_restrained_S_gt       ?
_refine_ls_restrained_S_all      ?
_refine_ls_number_reflns         1462
_refine_ls_number_parameters     55
_refine_ls_number_restraints     0
_refine_ls_number_constraints    23
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     w=1/(σ²(F)+0.0001F²)
_refine_ls_hydrogen_treatment    constr
_refine_ls_shift/su_max          0.0406
_refine_ls_shift/su_mean         0.0048
_refine_diff_density_max         5.39
_refine_diff_density_min         -1.85
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_extinction_expression ?
_refine_ls_abs_structure_details ?
_refine_ls_abs_structure_Flack   ?
_refine_ls_abs_structure_Rogers  ?

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0.0181 0.0091 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
H 0.0000 0.0000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
I -0.3257 6.8362 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
N 0.0311 0.0180 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
Pb -4.0753 8.5060 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'

_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_structure_solution    'Charge flipping'
_computing_structure_refinement  Jana2006
_computing_molecular_graphics    ?
_computing_publication_material  ?




#=======================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_adp_type
_atom_site_U_iso_or_equiv
_atom_site_site_symmetry_multiplicity
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.25 0.48500(6) 0.25 Uani 0.0372(3) 8 1 d . . .
I1 I 0.30025(10) 0 0 Uani 0.0617(6) 8 1 d . . .
I2 I 0.39977(5) 0.46930(9) 0.17577(10) Uani 0.0542(4) 16 1 d . . .
I3 I 0.25 0.23463(12) 0.25 Uani 0.0789(8) 8 1 d . . .
I4 I 0.5 0.14407(14) 0.11089(15) Uani 0.0745(8) 8 1 d . . .
N1 N 0.6236(11) 0.2682(16) -0.0258(15) Uani 0.088(8) 16 1 d . . .
C2 C 0.5 0.2608(18) -0.0187(15) Uani 0.053(9) 8 1 d . . .
C1 C 0.5598(12) 0.2453(15) -0.0837(18) Uani 0.088(10) 16 1 d . . .
H1n1 H 0.656751 0.246334 -0.065434 Uiso 0.1053 16 1 d . . .
H2n1 H 0.627164 0.335871 -0.015278 Uiso 0.1053 16 1 d . . .
H3n1 H 0.623942 0.235852 0.036891 Uiso 0.1053 16 1 d . . .
H1c2 H 0.5 0.331571 0.009132 Uiso 0.0637 8 1 d . . .
H1c1 H 0.560701 0.174484 -0.111392 Uiso 0.1061 16 1 d . . .
H2c1 H 0.557192 0.287293 -0.148921 Uiso 0.1061 16 1 d . . .


loop_
_jana_atom_site_ADP_C_label
_jana_atom_site_ADP_C_type_symbol
_jana_atom_site_ADP_C_111
_jana_atom_site_ADP_C_112
_jana_atom_site_ADP_C_113
_jana_atom_site_ADP_C_122
_jana_atom_site_ADP_C_123
_jana_atom_site_ADP_C_133
_jana_atom_site_ADP_C_222
_jana_atom_site_ADP_C_223
_jana_atom_site_ADP_C_233
_jana_atom_site_ADP_C_333
? ? ? ? ? ? ? ? ? ? ? ?

loop_
_jana_atom_site_ADP_D_label
_jana_atom_site_ADP_D_type_symbol
_jana_atom_site_ADP_D_1111
_jana_atom_site_ADP_D_1112
_jana_atom_site_ADP_D_1113
_jana_atom_site_ADP_D_1122
_jana_atom_site_ADP_D_1123
_jana_atom_site_ADP_D_1133
_jana_atom_site_ADP_D_1222
_jana_atom_site_ADP_D_1223
_jana_atom_site_ADP_D_1233
_jana_atom_site_ADP_D_1333
_jana_atom_site_ADP_D_2222
_jana_atom_site_ADP_D_2223
_jana_atom_site_ADP_D_2233
_jana_atom_site_ADP_D_2333
_jana_atom_site_ADP_D_3333
? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ?

loop_
_jana_atom_site_ADP_E_label
_jana_atom_site_ADP_E_type_symbol
_jana_atom_site_ADP_E_11111
_jana_atom_site_ADP_E_11112
_jana_atom_site_ADP_E_11113
_jana_atom_site_ADP_E_11122
_jana_atom_site_ADP_E_11123
_jana_atom_site_ADP_E_11133
_jana_atom_site_ADP_E_11222
_jana_atom_site_ADP_E_11223
_jana_atom_site_ADP_E_11233
_jana_atom_site_ADP_E_11333
_jana_atom_site_ADP_E_12222
_jana_atom_site_ADP_E_12223
_jana_atom_site_ADP_E_12233
_jana_atom_site_ADP_E_12333
_jana_atom_site_ADP_E_13333
_jana_atom_site_ADP_E_22222
_jana_atom_site_ADP_E_22223
_jana_atom_site_ADP_E_22233
_jana_atom_site_ADP_E_22333
_jana_atom_site_ADP_E_23333
_jana_atom_site_ADP_E_33333
? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ?

loop_
_jana_atom_site_ADP_F_label
_jana_atom_site_ADP_F_type_symbol
_jana_atom_site_ADP_F_111111
_jana_atom_site_ADP_F_111112
_jana_atom_site_ADP_F_111113
_jana_atom_site_ADP_F_111122
_jana_atom_site_ADP_F_111123
_jana_atom_site_ADP_F_111133
_jana_atom_site_ADP_F_111222
_jana_atom_site_ADP_F_111223
_jana_atom_site_ADP_F_111233
_jana_atom_site_ADP_F_111333
_jana_atom_site_ADP_F_112222
_jana_atom_site_ADP_F_112223
_jana_atom_site_ADP_F_112233
_jana_atom_site_ADP_F_112333
_jana_atom_site_ADP_F_113333
_jana_atom_site_ADP_F_122222
_jana_atom_site_ADP_F_122223
_jana_atom_site_ADP_F_122233
_jana_atom_site_ADP_F_122333
_jana_atom_site_ADP_F_123333
_jana_atom_site_ADP_F_133333
_jana_atom_site_ADP_F_222222
_jana_atom_site_ADP_F_222223
_jana_atom_site_ADP_F_222233
_jana_atom_site_ADP_F_222333
_jana_atom_site_ADP_F_223333
_jana_atom_site_ADP_F_233333
_jana_atom_site_ADP_F_333333
? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ?


#=======================================================================

# 10. MOLECULAR GEOMETRY


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pb1 I1 . 13_555 3.2250(7) ?
Pb1 I1 . 6_555 3.2250(7) ?
Pb1 I2 . . 3.1529(11) ?
Pb1 I2 . 11_555 3.1529(11) ?
Pb1 I3 . . 3.1736(18) ?
Pb1 I3 . 6_555 3.1643(18) ?
I1 N1 . 5_655 3.74(2) ?
I1 N1 . 8_655 3.74(2) ?
I2 N1 . 5_665 3.83(2) ?
I2 N1 . 8_655 3.577(19) ?
I3 N1 . 2_655 3.74(2) ?
I3 N1 . 12_455 3.74(2) ?
I4 N1 . . 3.38(2) ?
I4 N1 . 8_655 3.38(2) ?
I4 C2 . . 2.17(2) ?
N1 C1 . . 1.49(3) ?
N1 H1n1 . . 0.87(2) ?
N1 H2n1 . . 0.87(2) ?
N1 H3n1 . . 0.869(19) ?
C2 C1 . . 1.46(3) ?
C2 C1 . 8_655 1.46(3) ?
C2 H1c2 . . 0.96(2) ?
C1 H1c1 . . 0.960(19) ?
C1 H2c1 . . 0.96(2) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
I1 Pb1 I1 13_555 . 6_555 173.24(3) ?
I1 Pb1 I2 13_555 . . 91.74(4) ?
I1 Pb1 I2 13_555 . 11_555 88.68(4) ?
I1 Pb1 I3 13_555 . . 93.380(14) ?
I1 Pb1 I3 13_555 . 6_555 86.620(14) ?
I1 Pb1 I2 6_555 . . 88.68(4) ?
I1 Pb1 I2 6_555 . 11_555 91.74(4) ?
I1 Pb1 I3 6_555 . . 93.380(14) ?
I1 Pb1 I3 6_555 . 6_555 86.620(14) ?
I2 Pb1 I2 . . 11_555 172.76(4) ?
I2 Pb1 I3 . . . 86.38(2) ?
I2 Pb1 I3 . . 6_555 93.62(2) ?
I2 Pb1 I3 11_555 . . 86.38(2) ?
I2 Pb1 I3 11_555 . 6_555 93.62(2) ?
I3 Pb1 I3 . . 6_555 180 ?
Pb1 I1 Pb1 13_555 . 6_545 143.47(7) ?
Pb1 I1 N1 13_555 . 5_655 105.2(3) ?
Pb1 I1 N1 13_555 . 8_655 89.7(3) ?
Pb1 I1 N1 6_545 . 5_655 89.7(3) ?
Pb1 I1 N1 6_545 . 8_655 105.2(3) ?
N1 I1 N1 5_655 . 8_655 131.7(5) ?
Pb1 I2 N1 . . 5_665 88.0(3) ?
Pb1 I2 N1 . . 8_655 96.8(4) ?
N1 I2 N1 5_665 . 8_655 105.9(4) ?
Pb1 I3 Pb1 . . 6_545 180 ?
Pb1 I3 N1 . . 2_655 90.5(3) ?
Pb1 I3 N1 . . 12_455 90.5(3) ?
Pb1 I3 N1 6_545 . 2_655 89.5(3) ?
Pb1 I3 N1 6_545 . 12_455 89.5(3) ?
N1 I3 N1 2_655 . 12_455 178.9(4) ?
N1 I4 N1 . . 8_655 94.6(5) ?
N1 I4 C2 . . . 47.3(4) ?
N1 I4 C2 8_655 . . 47.3(4) ?
I1 N1 I2 5_655 . 5_665 151.7(6) ?
I1 N1 I2 5_655 . 8_655 130.0(5) ?
I1 N1 I3 5_655 . 2_654 77.0(4) ?
I1 N1 I4 5_655 . . 80.6(4) ?
I1 N1 C1 5_655 . . 102.4(12) ?
I1 N1 H1n1 5_655 . . 56.2(12) ?
I1 N1 H2n1 5_655 . . 148.1(17) ?
I1 N1 H3n1 5_655 . . 59.6(12) ?
I2 N1 I2 5_665 . 8_655 72.2(4) ?
I2 N1 I3 5_665 . 2_654 75.0(4) ?
I2 N1 I4 5_665 . . 123.4(6) ?
I2 N1 C1 5_665 . . 80.6(11) ?
I2 N1 H1n1 5_665 . . 96.0(13) ?
I2 N1 H2n1 5_665 . . 39.1(10) ?
I2 N1 H3n1 5_665 . . 146.4(16) ?
I2 N1 I3 8_655 . 2_654 127.0(6) ?
I2 N1 I4 8_655 . . 83.9(4) ?
I2 N1 C1 8_655 . . 110.6(13) ?
I2 N1 H1n1 8_655 . . 135.4(16) ?
I2 N1 H2n1 8_655 . . 37.5(10) ?
I2 N1 H3n1 8_655 . . 74.3(12) ?
I3 N1 I4 2_654 . . 149.0(6) ?
I3 N1 C1 2_654 . . 103.6(12) ?
I3 N1 H1n1 2_654 . . 21.1(10) ?
I3 N1 H2n1 2_654 . . 93.5(14) ?
I3 N1 H3n1 2_654 . . 129.5(17) ?
I4 N1 C1 . . . 60.8(11) ?
I4 N1 H1n1 . . . 133.7(16) ?
I4 N1 H2n1 . . . 116.5(15) ?
I4 N1 H3n1 . . . 49.5(12) ?
C1 N1 H1n1 . . . 109.4(18) ?
C1 N1 H2n1 . . . 109(2) ?
C1 N1 H3n1 . . . 109(2) ?
H1n1 N1 H2n1 . . . 109(2) ?
H1n1 N1 H3n1 . . . 110(2) ?
H2n1 N1 H3n1 . . . 110(2) ?
I4 C2 C1 . . . 107.9(12) ?
I4 C2 C1 . . 8_655 107.9(12) ?
I4 C2 H1c2 . . . 112.3(14) ?
C1 C2 C1 . . 8_655 111.5(17) ?
C1 C2 H1c2 . . . 108.7(14) ?
C1 C2 H1c2 8_655 . . 108.7(14) ?
N1 C1 C2 . . . 115.2(17) ?
N1 C1 H1c1 . . . 109(2) ?
N1 C1 H2c1 . . . 109(2) ?
C2 C1 H1c1 . . . 110(2) ?
C2 C1 H2c1 . . . 109(2) ?
H1c1 C1 H2c1 . . . 103(2) ?

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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
? ? ? ? ? ? ? ? ? ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
? ? ? ? ? ? ? ? ? ? ?


#=======================================================================

# 11. STRUCTURE-FACTOR LIST



####################################################################### 
# 
# 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_n=2_(DicI)MAPb2I7
_database_code_depnum_ccdc_archive 'CCDC 2283259'
loop_
_audit_author_name
_audit_author_address
'Nicolas Mercier'
;UNIV Angers, UMR CNRS
France
;
_audit_update_record             
;
2023-11-24 deposited with the CCDC.	2023-11-30 downloaded from the CCDC.
;
#=======================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic        
; ?
;
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_iupac          ?
_chemical_formula_sum            'C4 H17 I8 N3 Pb2'
_chemical_formula_weight         1536.8
_chemical_melting_point          ?
_chemical_compound_source        ?
_chemical_absolute_configuration .

#=======================================================================

# 6. CRYSTAL DATA

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b a m'
_symmetry_space_group_name_Hall  '-P -2xab;-2yab;-2z'
_symmetry_Int_Tables_number      55

loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,-y,z
3 -x+1/2,y+1/2,-z
4 x+1/2,-y+1/2,-z
5 -x,-y,-z
6 x,y,-z
7 x+1/2,-y+1/2,z
8 -x+1/2,y+1/2,z

_cell_length_a                   12.3289(8)
_cell_length_b                   12.7636(7)
_cell_length_c                   16.2040(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2549.9(3)


_cell_formula_units_Z            4

_cell_measurement_reflns_used    4733
_cell_measurement_theta_min      2.67
_cell_measurement_theta_max      70.79
_cell_measurement_temperature    293
_cell_special_details            
; ?
;

_exptl_crystal_density_diffrn    4.0032
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             2600

_exptl_absorpt_coefficient_mu    101.352
_exptl_crystal_description       'elongated parallelepipeds'
_exptl_crystal_size_max          0.063
_exptl_crystal_size_mid          0.048
_exptl_crystal_size_min          0.020
_exptl_crystal_size_rad          ?
_exptl_crystal_colour            red
_exptl_absorpt_correction_type   multi-scan
_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_absorpt_correction_T_min  0.485
_exptl_absorpt_correction_T_max  1
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
? ? ? ?

#=======================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           ?


_diffrn_ambient_temperature      293
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_power             ?
_diffrn_source_voltage           ?
_diffrn_source_current           ?
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'SuperNova, Single source at offset/far, AtlasS2'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1990
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support ?


_diffrn_reflns_number            19812
_diffrn_reflns_theta_min         2.73
_diffrn_reflns_theta_max         71.27
_diffrn_reflns_theta_full        71.27
_diffrn_measured_fraction_theta_max 1
_diffrn_measured_fraction_theta_full 1
_diffrn_reflns_av_R_equivalents  0.0789
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_reduction_process ?

_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?

_diffrn_radiation_probe          X-ray

#=======================================================================

# 8. REFINEMENT DATA

_refine_special_details          
; ?
;

_reflns_number_total             2398
_reflns_number_gt                1874
_reflns_threshold_expression     I>2σ(I)

_refine_ls_structure_factor_coef F
_refine_ls_R_factor_gt           0.0311
_refine_ls_wR_factor_gt          0.0329
_refine_ls_R_factor_all          0.0451
_refine_ls_wR_factor_ref         0.0349
_refine_ls_goodness_of_fit_ref   1.08
_refine_ls_goodness_of_fit_gt    1.16
_refine_ls_restrained_S_gt       ?
_refine_ls_restrained_S_all      ?
_refine_ls_number_reflns         2398
_refine_ls_number_parameters     86
_refine_ls_number_restraints     0
_refine_ls_number_constraints    47
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     w=1/(σ²(F)+0.0001F²)
_refine_ls_hydrogen_treatment    constr
_refine_ls_shift/su_max          0.0336
_refine_ls_shift/su_mean         0.0021
_refine_diff_density_max         4.77
_refine_diff_density_min         -1.24
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_extinction_expression ?
_refine_ls_abs_structure_details ?
_refine_ls_abs_structure_Flack   ?
_refine_ls_abs_structure_Rogers  ?

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0.0181 0.0091 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
H 0.0000 0.0000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
I -0.3257 6.8362 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
N 0.0311 0.0180 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
Pb -4.0753 8.5060 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'

_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_structure_solution    'Charge flipping'
_computing_structure_refinement  Jana2006
_computing_molecular_graphics    ?
_computing_publication_material  ?



#=======================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_adp_type
_atom_site_U_iso_or_equiv
_atom_site_site_symmetry_multiplicity
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.75060(3) 0.01280(3) 0.30164(2) Uani 0.02863(12) 8 1 d . . .
I1 I 0.82320(6) 0.02809(5) 0.12084(4) Uani 0.0400(2) 8 1 d . . .
I2 I 0.5 0 0.24417(7) Uani 0.0493(4) 4 1 d . . .
I3 I 0.24831(7) 0.23713(5) 0.29989(5) Uani 0.0526(3) 8 1 d . . .
I4 I 0 0 0.35300(7) Uani 0.0574(4) 4 1 d . . .
I5 I 0.70042(10) 0.01448(9) 0.5 Uani 0.0565(4) 4 1 d . . .
I6 I 0.38374(9) 0.14607(9) 0 Uani 0.0581(4) 4 1 d . . .
N1 N 0.0227(8) 0.2330(8) 0.1525(7) Uani 0.061(4) 8 1 d . . .
C2 C 0.5146(10) 0.2574(10) 0 Uani 0.036(5) 4 1 d . . .
N2 N -0.0211(19) 0.259(2) 0.5 Uani 0.168(19) 4 1 d . . .
C3 C 0.0799(17) 0.2136(17) 0.5 Uani 0.078(9) 4 1 d . . .
C1 C 0.0848(10) 0.2549(8) 0.0755(8) Uani 0.059(5) 8 1 d . . .
H1n1 H 0.065634 0.238258 0.194865 Uiso 0.0731 8 1 d . . .
H2n1 H -0.029948 0.277968 0.157183 Uiso 0.0731 8 1 d . . .
H3n1 H -0.003906 0.169893 0.150279 Uiso 0.0731 8 1 d . . .
H1c2 H 0.482138 0.325813 0 Uiso 0.0437 4 1 d . . .
H1n2 H -0.025082 0.304602 0.459984 Uiso 0.2014 8 0.5 d . . .
H2n2 H -0.070378 0.211321 0.49316 Uiso 0.2014 8 0.5 d . . .
H3n2 H -0.031695 0.290984 0.546856 Uiso 0.2014 8 0.5 d . . .
H1c3 H 0.100274 0.196582 0.444418 Uiso 0.0931 8 0.5 d . . .
H2c3 H 0.131768 0.26144 0.523003 Uiso 0.0931 8 0.5 d . . .
H3c3 H 0.078037 0.150787 0.532579 Uiso 0.0931 8 0.5 d . . .
H1c1 H 0.145452 0.207863 0.071958 Uiso 0.0706 8 1 d . . .
H2c1 H 0.11315 0.324887 0.077515 Uiso 0.0706 8 1 d . . .


loop_
_jana_atom_site_ADP_C_label
_jana_atom_site_ADP_C_type_symbol
_jana_atom_site_ADP_C_111
_jana_atom_site_ADP_C_112
_jana_atom_site_ADP_C_113
_jana_atom_site_ADP_C_122
_jana_atom_site_ADP_C_123
_jana_atom_site_ADP_C_133
_jana_atom_site_ADP_C_222
_jana_atom_site_ADP_C_223
_jana_atom_site_ADP_C_233
_jana_atom_site_ADP_C_333
? ? ? ? ? ? ? ? ? ? ? ?

loop_
_jana_atom_site_ADP_D_label
_jana_atom_site_ADP_D_type_symbol
_jana_atom_site_ADP_D_1111
_jana_atom_site_ADP_D_1112
_jana_atom_site_ADP_D_1113
_jana_atom_site_ADP_D_1122
_jana_atom_site_ADP_D_1123
_jana_atom_site_ADP_D_1133
_jana_atom_site_ADP_D_1222
_jana_atom_site_ADP_D_1223
_jana_atom_site_ADP_D_1233
_jana_atom_site_ADP_D_1333
_jana_atom_site_ADP_D_2222
_jana_atom_site_ADP_D_2223
_jana_atom_site_ADP_D_2233
_jana_atom_site_ADP_D_2333
_jana_atom_site_ADP_D_3333
? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ?

loop_
_jana_atom_site_ADP_E_label
_jana_atom_site_ADP_E_type_symbol
_jana_atom_site_ADP_E_11111
_jana_atom_site_ADP_E_11112
_jana_atom_site_ADP_E_11113
_jana_atom_site_ADP_E_11122
_jana_atom_site_ADP_E_11123
_jana_atom_site_ADP_E_11133
_jana_atom_site_ADP_E_11222
_jana_atom_site_ADP_E_11223
_jana_atom_site_ADP_E_11233
_jana_atom_site_ADP_E_11333
_jana_atom_site_ADP_E_12222
_jana_atom_site_ADP_E_12223
_jana_atom_site_ADP_E_12233
_jana_atom_site_ADP_E_12333
_jana_atom_site_ADP_E_13333
_jana_atom_site_ADP_E_22222
_jana_atom_site_ADP_E_22223
_jana_atom_site_ADP_E_22233
_jana_atom_site_ADP_E_22333
_jana_atom_site_ADP_E_23333
_jana_atom_site_ADP_E_33333
? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ?

loop_
_jana_atom_site_ADP_F_label
_jana_atom_site_ADP_F_type_symbol
_jana_atom_site_ADP_F_111111
_jana_atom_site_ADP_F_111112
_jana_atom_site_ADP_F_111113
_jana_atom_site_ADP_F_111122
_jana_atom_site_ADP_F_111123
_jana_atom_site_ADP_F_111133
_jana_atom_site_ADP_F_111222
_jana_atom_site_ADP_F_111223
_jana_atom_site_ADP_F_111233
_jana_atom_site_ADP_F_111333
_jana_atom_site_ADP_F_112222
_jana_atom_site_ADP_F_112223
_jana_atom_site_ADP_F_112233
_jana_atom_site_ADP_F_112333
_jana_atom_site_ADP_F_113333
_jana_atom_site_ADP_F_122222
_jana_atom_site_ADP_F_122223
_jana_atom_site_ADP_F_122233
_jana_atom_site_ADP_F_122333
_jana_atom_site_ADP_F_123333
_jana_atom_site_ADP_F_133333
_jana_atom_site_ADP_F_222222
_jana_atom_site_ADP_F_222223
_jana_atom_site_ADP_F_222233
_jana_atom_site_ADP_F_222333
_jana_atom_site_ADP_F_223333
_jana_atom_site_ADP_F_233333
_jana_atom_site_ADP_F_333333
? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ?


#=======================================================================

# 10. MOLECULAR GEOMETRY


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pb1 I1 . . 3.0696(8) ?
Pb1 I2 . . 3.2310(6) ?
Pb1 I3 . 2_655 3.1902(8) ?
Pb1 I3 . 7_555 3.1920(8) ?
Pb1 I4 . 1_655 3.1897(6) ?
Pb1 I5 . . 3.2733(5) ?
I1 N1 . 1_655 3.627(10) ?
I1 N1 . 2_655 3.870(10) ?
I2 N1 . 7_555 3.728(10) ?
I2 N1 . 8_545 3.728(10) ?
I3 N1 . . 3.667(11) ?
I3 N1 . 7_555 4.159(10) ?
I4 N2 . . 4.08(2) ?
I4 N2 . 2_555 4.08(2) ?
I5 N2 . 3_546 3.94(2) ?
I5 N2 . 4_556 3.98(2) ?
I6 N1 . 4_555 3.380(11) ?
I6 N1 . 7_555 3.380(11) ?
I6 C2 . . 2.150(13) ?
N1 C1 . . 1.490(17) ?
N1 H1n1 . . 0.869(11) ?
N1 H2n1 . . 0.870(10) ?
N1 H3n1 . . 0.870(10) ?
C2 C1 . 4_555 1.507(15) ?
C2 C1 . 7_555 1.507(15) ?
C2 H1c2 . . 0.961(13) ?
N2 C3 . . 1.37(3) ?
N2 H1n2 . . 0.873(17) ?
N2 H1n2 . 6_556 0.873(17) ?
N2 H2n2 . . 0.87(2) ?
N2 H2n2 . 6_556 0.87(2) ?
N2 H3n2 . . 0.872(12) ?
N2 H3n2 . 6_556 0.872(12) ?
C3 H1c3 . . 0.960(7) ?
C3 H1c3 . 6_556 0.960(7) ?
C3 H2c3 . . 0.96(2) ?
C3 H2c3 . 6_556 0.96(2) ?
C3 H3c3 . . 0.960(18) ?
C3 H3c3 . 6_556 0.960(18) ?
C1 H1c1 . . 0.961(12) ?
C1 H2c1 . . 0.960(11) ?
H1n2 H3n2 . 6_556 0.221683(17) ?
H2n2 H2n2 . 6_556 0.22167(2) ?
H1c3 H3c3 . 6_556 0.74549(6) ?
H2c3 H2c3 . 6_556 0.74548(8) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
I1 Pb1 I2 . . . 90.40(3) ?
I1 Pb1 I3 . . 2_655 93.09(2) ?
I1 Pb1 I3 . . 7_555 86.02(2) ?
I1 Pb1 I4 . . 1_655 88.35(3) ?
I1 Pb1 I5 . . . 172.70(3) ?
I2 Pb1 I3 . . 2_655 87.186(18) ?
I2 Pb1 I3 . . 7_555 92.266(18) ?
I2 Pb1 I4 . . 1_655 173.943(15) ?
I2 Pb1 I5 . . . 95.89(3) ?
I3 Pb1 I3 2_655 . 7_555 178.95(2) ?
I3 Pb1 I4 2_655 . 1_655 86.964(18) ?
I3 Pb1 I5 2_655 . . 90.92(3) ?
I3 Pb1 I4 7_555 . 1_655 93.558(18) ?
I3 Pb1 I5 7_555 . . 90.03(3) ?
I4 Pb1 I5 1_655 . . 85.77(3) ?
Pb1 I1 N1 . . 1_655 96.23(18) ?
Pb1 I1 N1 . . 2_655 87.82(17) ?
N1 I1 N1 1_655 . 2_655 105.6(2) ?
Pb1 I2 Pb1 . . 2_655 146.50(4) ?
Pb1 I2 N1 . . 7_555 89.82(15) ?
Pb1 I2 N1 . . 8_545 103.46(15) ?
Pb1 I2 N1 2_655 . 7_555 103.46(15) ?
Pb1 I2 N1 2_655 . 8_545 89.82(15) ?
N1 I2 N1 7_555 . 8_545 133.0(2) ?
Pb1 I3 Pb1 2_655 . 7_455 178.74(3) ?
Pb1 I3 N1 2_655 . . 89.69(16) ?
Pb1 I3 N1 2_655 . 7_555 95.36(14) ?
Pb1 I3 N1 7_455 . . 91.54(16) ?
Pb1 I3 N1 7_455 . 7_555 84.62(14) ?
N1 I3 N1 . . 7_555 104.1(2) ?
Pb1 I4 Pb1 1_455 . 2_655 149.75(4) ?
Pb1 I4 N2 1_455 . . 92.8(3) ?
Pb1 I4 N2 1_455 . 2_555 104.8(3) ?
Pb1 I4 N2 2_655 . . 104.8(3) ?
Pb1 I4 N2 2_655 . 2_555 92.8(3) ?
N2 I4 N2 . . 2_555 108.6(3) ?
Pb1 I5 Pb1 . . 6_556 158.20(4) ?
Pb1 I5 N2 . . 3_546 95.78(6) ?
Pb1 I5 N2 . . 4_556 97.73(5) ?
Pb1 I5 N2 6_556 . 3_546 95.78(6) ?
Pb1 I5 N2 6_556 . 4_556 97.73(5) ?
N2 I5 N2 3_546 . 4_556 102.5(5) ?
N1 I6 N1 4_555 . 7_555 94.0(3) ?
N1 I6 C2 4_555 . . 46.98(18) ?
N1 I6 C2 7_555 . . 46.98(18) ?
I1 N1 I1 1_455 . 2_655 72.14(19) ?
I1 N1 I2 1_455 . 7_455 131.7(3) ?
I1 N1 I3 1_455 . . 128.1(3) ?
I1 N1 I3 1_455 . 7_455 66.15(16) ?
I1 N1 I6 1_455 . 4_455 83.2(2) ?
I1 N1 C1 1_455 . . 111.4(7) ?
I1 N1 H1n1 1_455 . . 125.5(8) ?
I1 N1 H2n1 1_455 . . 89.0(7) ?
I1 N1 H3n1 1_455 . . 21.8(5) ?
I1 N1 I2 2_655 . 7_455 151.3(3) ?
I1 N1 I3 2_655 . . 74.12(19) ?
I1 N1 I3 2_655 . 7_455 123.7(3) ?
I1 N1 I6 2_655 . 4_455 123.0(3) ?
I1 N1 C1 2_655 . . 78.4(6) ?
I1 N1 H1n1 2_655 . . 82.7(7) ?
I1 N1 H2n1 2_655 . . 161.1(8) ?
I1 N1 H3n1 2_655 . . 51.9(6) ?
I2 N1 I3 7_455 . . 77.5(2) ?
I2 N1 I3 7_455 . 7_455 68.06(17) ?
I2 N1 I6 7_455 . 4_455 80.5(2) ?
I2 N1 C1 7_455 . . 101.6(6) ?
I2 N1 H1n1 7_455 . . 70.2(6) ?
I2 N1 H2n1 7_455 . . 46.1(6) ?
I2 N1 H3n1 7_455 . . 146.5(8) ?
I3 N1 I3 . . 7_455 104.0(3) ?
I3 N1 I6 . . 4_455 148.7(3) ?
I3 N1 C1 . . . 98.8(6) ?
I3 N1 H1n1 . . . 12.2(5) ?
I3 N1 H2n1 . . . 120.0(8) ?
I3 N1 H3n1 . . . 109.0(8) ?
I3 N1 I6 7_455 . 4_455 88.0(2) ?
I3 N1 C1 7_455 . . 151.8(7) ?
I3 N1 H1n1 7_455 . . 92.0(7) ?
I3 N1 H2n1 7_455 . . 44.1(6) ?
I3 N1 H3n1 7_455 . . 78.6(7) ?
I6 N1 C1 4_455 . . 64.1(6) ?
I6 N1 H1n1 4_455 . . 148.3(8) ?
I6 N1 H2n1 4_455 . . 52.0(6) ?
I6 N1 H3n1 4_455 . . 101.6(8) ?
C1 N1 H1n1 . . . 109.5(10) ?
C1 N1 H2n1 . . . 109.4(10) ?
C1 N1 H3n1 . . . 109.4(10) ?
H1n1 N1 H2n1 . . . 109.5(12) ?
H1n1 N1 H3n1 . . . 109.5(11) ?
H2n1 N1 H3n1 . . . 109.5(11) ?
I6 C2 C1 . . 4_555 111.2(7) ?
I6 C2 C1 . . 7_555 111.2(7) ?
I6 C2 H1c2 . . . 106.7(9) ?
C1 C2 C1 4_555 . 7_555 108.6(10) ?
C1 C2 H1c2 4_555 . . 109.5(8) ?
C1 C2 H1c2 7_555 . . 109.5(8) ?
I4 N2 I4 . . 5_556 71.4(4) ?
I4 N2 I5 . . 3_556 134.9(4) ?
I4 N2 I5 . . 4_456 123.0(5) ?
I4 N2 C3 . . . 66.5(10) ?
I4 N2 H1n2 . . . 96.3(10) ?
I4 N2 H1n2 . . 6_556 167.7(15) ?
I4 N2 H2n2 . . . 53.3(11) ?
I4 N2 H2n2 . . 6_556 63.3(11) ?
I4 N2 H3n2 . . . 153.7(17) ?
I4 N2 H3n2 . . 6_556 83.1(13) ?
I4 N2 I5 5_556 . 3_556 134.9(4) ?
I4 N2 I5 5_556 . 4_456 123.0(5) ?
I4 N2 C3 5_556 . . 66.5(10) ?
I4 N2 H1n2 5_556 . . 167.7(15) ?
I4 N2 H1n2 5_556 . 6_556 96.3(10) ?
I4 N2 H2n2 5_556 . . 63.3(11) ?
I4 N2 H2n2 5_556 . 6_556 53.3(11) ?
I4 N2 H3n2 5_556 . . 83.1(13) ?
I4 N2 H3n2 5_556 . 6_556 153.7(17) ?
I5 N2 I5 3_556 . 4_456 77.5(5) ?
I5 N2 C3 3_556 . . 149.1(16) ?
I5 N2 H1n2 3_556 . . 54.3(13) ?
I5 N2 H1n2 3_556 . 6_556 54.3(13) ?
I5 N2 H2n2 3_556 . . 100.8(17) ?
I5 N2 H2n2 3_556 . 6_556 100.8(17) ?
I5 N2 H3n2 3_556 . . 61.9(14) ?
I5 N2 H3n2 3_556 . 6_556 61.9(14) ?
I5 N2 C3 4_456 . . 71.6(13) ?
I5 N2 H1n2 4_456 . . 63.5(14) ?
I5 N2 H1n2 4_456 . 6_556 63.5(14) ?
I5 N2 H2n2 4_456 . . 172.5(5) ?
I5 N2 H2n2 4_456 . 6_556 172.5(5) ?
I5 N2 H3n2 4_456 . . 76.3(16) ?
I5 N2 H3n2 4_456 . 6_556 76.3(16) ?
C3 N2 H1n2 . . . 109.4(18) ?
C3 N2 H1n2 . . 6_556 109.4(18) ?
C3 N2 H2n2 . . . 110(2) ?
C3 N2 H2n2 . . 6_556 110(2) ?
C3 N2 H3n2 . . . 109.5(16) ?
C3 N2 H3n2 . . 6_556 109.5(16) ?
H1n2 N2 H1n2 . . 6_556 96(2) ?
H1n2 N2 H2n2 . . . 109.5(17) ?
H1n2 N2 H2n2 . . 6_556 122(2) ?
H1n2 N2 H3n2 . . . 109(3) ?
H1n2 N2 H3n2 . . 6_556 14.6(2) ?
H1n2 N2 H2n2 6_556 . . 122(2) ?
H1n2 N2 H2n2 6_556 . 6_556 109.5(17) ?
H1n2 N2 H3n2 6_556 . . 14.6(2) ?
H1n2 N2 H3n2 6_556 . 6_556 109(3) ?
H2n2 N2 H2n2 . . 6_556 14.7(4) ?
H2n2 N2 H3n2 . . . 109.6(19) ?
H2n2 N2 H3n2 . . 6_556 96.4(15) ?
H2n2 N2 H3n2 6_556 . . 96.4(15) ?
H2n2 N2 H3n2 6_556 . 6_556 109.6(19) ?
H3n2 N2 H3n2 . . 6_556 121(3) ?
N2 C3 H1c3 . . . 109.4(12) ?
N2 C3 H1c3 . . 6_556 109.4(12) ?
N2 C3 H2c3 . . . 110(2) ?
N2 C3 H2c3 . . 6_556 110(2) ?
N2 C3 H3c3 . . . 109.3(18) ?
N2 C3 H3c3 . . 6_556 109.3(18) ?
H1c3 C3 H1c3 . . 6_556 140(2) ?
H1c3 C3 H2c3 . . . 109.5(18) ?
H1c3 C3 H2c3 . . 6_556 66.7(8) ?
H1c3 C3 H3c3 . . . 109(2) ?
H1c3 C3 H3c3 . . 6_556 45.7(6) ?
H1c3 C3 H2c3 6_556 . . 66.7(8) ?
H1c3 C3 H2c3 6_556 . 6_556 109.5(18) ?
H1c3 C3 H3c3 6_556 . . 45.7(6) ?
H1c3 C3 H3c3 6_556 . 6_556 109(2) ?
H2c3 C3 H2c3 . . 6_556 45.7(10) ?
H2c3 C3 H3c3 . . . 109.5(12) ?
H2c3 C3 H3c3 . . 6_556 140(2) ?
H2c3 C3 H3c3 6_556 . . 140(2) ?
H2c3 C3 H3c3 6_556 . 6_556 109.5(12) ?
H3c3 C3 H3c3 . . 6_556 66.7(14) ?
N1 C1 C2 . . 4_455 111.4(9) ?
N1 C1 H1c1 . . . 109.4(10) ?
N1 C1 H2c1 . . . 109.5(11) ?
C2 C1 H1c1 4_455 . . 109.5(11) ?
C2 C1 H2c1 4_455 . . 109.5(11) ?
H1c1 C1 H2c1 . . . 107.5(12) ?
N2 H1n2 H3n2 . . 6_556 82.5(13) ?
N2 H2n2 H2n2 . . 6_556 82.7(2) ?
N2 H3n2 H1n2 . . 6_556 82.9(15) ?
C3 H1c3 H3c3 . . 6_556 67.2(13) ?
C3 H2c3 H2c3 . . 6_556 67.1(5) ?
C3 H3c3 H1c3 . . 6_556 67.1(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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
? ? ? ? ? ? ? ? ? ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
? ? ? ? ? ? ? ? ? ? ?


#=======================================================================

# 11. STRUCTURE-FACTOR LIST



####################################################################### 
# 
# 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_n=3_(DicI)(MA)2Pb3I10
_database_code_depnum_ccdc_archive 'CCDC 2283266'
loop_
_audit_author_name
_audit_author_address
'Nicolas Mercier'
;UNIV Angers, UMR CNRS
France
;
_audit_update_record             
;
2023-11-24 deposited with the CCDC.	2023-11-30 downloaded from the CCDC.
;
#=======================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic        
; ?
;
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_iupac          ?
_chemical_formula_sum            'C5 H23 I11 N4 Pb3'
_chemical_formula_weight         2156.8
_chemical_melting_point          ?
_chemical_compound_source        ?
_chemical_absolute_configuration ?

#=======================================================================

# 6. CRYSTAL DATA

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'A e a 2'
_symmetry_space_group_name_Hall  'A -2xab;-2yab;2z'
_symmetry_Int_Tables_number      41

loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,-y,z
3 x+1/2,-y,z+1/2
4 -x+1/2,y,z+1/2
5 x,y+1/2,z+1/2
6 -x,-y+1/2,z+1/2
7 x+1/2,-y+1/2,z
8 -x+1/2,y+1/2,z

_cell_length_a                   12.3926(5)
_cell_length_b                   12.7378(5)
_cell_length_c                   44.8986(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7087.4(5)

loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.42(5) 1 0 0 0 1 0 0 0 1
2 0.58(5) -1 0 0 0 -1 0 0 0 -1

_cell_formula_units_Z            8

_cell_measurement_reflns_used    7801
_cell_measurement_theta_min      3.94
_cell_measurement_theta_max      70.87
_cell_measurement_temperature    260(50)
_cell_special_details            
; ?
;

_exptl_crystal_density_diffrn    4.0426
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             7280

_exptl_absorpt_coefficient_mu    102.52
_exptl_crystal_description       'plate like crystals'
_exptl_crystal_size_max          0.105
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.032
_exptl_crystal_size_rad          ?
_exptl_crystal_colour            black
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.71a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.062
_exptl_absorpt_correction_T_max  1
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
? ? ? ?

#=======================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           ?


_diffrn_ambient_temperature      255
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_power             ?
_diffrn_source_voltage           ?
_diffrn_source_current           ?
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'SuperNova, Single source at offset/far, AtlasS2'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1990
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support ?


_diffrn_reflns_number            27401
_diffrn_reflns_theta_min         3.94
_diffrn_reflns_theta_max         71.97
_diffrn_reflns_theta_full        71.97
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measured_fraction_theta_full 0.99
_diffrn_reflns_av_R_equivalents  0.0732
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_reduction_process ?

_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?

_diffrn_radiation_probe          X-ray

#=======================================================================

# 8. REFINEMENT DATA

_refine_special_details          
; ?
;

_reflns_number_total             6181
_reflns_number_gt                4798
_reflns_threshold_expression     I>2σ(I)

_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_gt           0.0533
_refine_ls_wR_factor_gt          0.1129
_refine_ls_R_factor_all          0.0668
_refine_ls_wR_factor_ref         0.1180
_refine_ls_goodness_of_fit_ref   1.71
_refine_ls_goodness_of_fit_gt    1.87
_refine_ls_restrained_S_gt       ?
_refine_ls_restrained_S_all      ?
_refine_ls_number_reflns         6181
_refine_ls_number_parameters     176
_refine_ls_number_restraints     9
_refine_ls_number_constraints    129
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     w=1/(σ²(I)+0.0004I²)
_refine_ls_hydrogen_treatment    constr
_refine_ls_shift/su_max          0.0445
_refine_ls_shift/su_mean         0.0041
_refine_diff_density_max         4.78
_refine_diff_density_min         -1.72
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_extinction_expression ?
_refine_ls_abs_structure_details 
;  2923 of Friedel pairs used in the refinement
;
_refine_ls_abs_structure_Flack   0.58(5)
_refine_ls_abs_structure_Rogers  ?

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0.0181 0.0091 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
H 0.0000 0.0000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
I -0.3257 6.8362 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
N 0.0311 0.0180 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
Pb -4.0753 8.5060 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'

_computing_data_collection       'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_computing_structure_solution    'Charge flipping'
_computing_structure_refinement  Jana2006
_computing_molecular_graphics    ?
_computing_publication_material  ?

loop_
_restr_distance_atom_site_label_1
_restr_distance_site_symmetry_1
_restr_distance_atom_site_label_2
_restr_distance_site_symmetry_2
_restr_distance_target
_restr_distance_target_weight_param
C1 . N1 . 1.48 0.001
C2 . N2 . 1.48 0.001
C5 . N4 . 1.48 0.001
N3 . C4 . 1.48 0.001
C5 . C3 . 1.52 0.001
C3 . C4 . 1.52 0.001

loop_
_restr_angle_atom_site_label_1
_restr_angle_site_symmetry_1
_restr_angle_atom_site_label_2
_restr_angle_site_symmetry_2
_restr_angle_atom_site_label_3
_restr_angle_site_symmetry_3
_restr_angle_target
_restr_angle_target_weight_param
N4 . C5 . C3 . 109.47 0.01
C5 . C3 . C4 . 109.47 0.01
C3 . C4 . N3 . 109.47 0.01



#=======================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_adp_type
_atom_site_U_iso_or_equiv
_atom_site_site_symmetry_multiplicity
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.5 0 0.22497(11) Uani 0.071(2) 4 1 d . . .
I2 I 0 0 0.43968(14) Uani 0.0565(19) 4 1 d . . .
I3 I 0 0 0.08737(13) Uani 0.074(2) 4 1 d . . .
Pb1 Pb 0.25186(15) 0.51032(16) 0.74295(5) Uani 0.0307(6) 8 1 d . . .
Pb2 Pb 0.2496(2) 0.50474(4) 0.60101(7) Uani 0.02978(17) 8 1 d . . .
Pb3 Pb 0.75161(15) 0.49080(17) 0.45937(5) Uani 0.0301(6) 8 1 d . . .
I4 I 0.7033(5) 0.4918(4) 0.53095(7) Uani 0.0637(15) 8 1 d . . .
I5 I 0.3241(3) 0.5245(3) 0.80750(7) Uani 0.0452(11) 8 1 d . . .
I6 I 0.3213(3) 0.0258(3) 0.39395(8) Uani 0.0489(12) 8 1 d . . .
I7 I 0.2019(5) 0.5064(4) 0.66993(7) Uani 0.0632(15) 8 1 d . . .
I8 I 0.7500(5) 0.2388(3) 0.24389(13) Uani 0.0561(14) 8 1 d . . .
I9 I 0.88275(11) 0.14768(11) 0.35101(17) Uani 0.0679(5) 8 1 d . . .
I10 I 0.2503(7) 0.25409(9) 0.10179(16) Uani 0.0595(5) 8 1 d . . .
I11 I 0.7493(5) 0.2406(3) 0.45925(13) Uani 0.0607(15) 8 1 d . . .
I12 I 0.5 0 0.11615(13) Uani 0.0561(16) 4 1 d . . .
I13 I 0 0.5 0.76228(13) Uani 0.0525(18) 4 1 d . . .
I14 I 0.5 0 0.47727(11) Uani 0.0560(18) 4 1 d . . .
N1 N 0.428(2) -0.214(3) 0.5319(7) Uani 0.110(13) 8 1 d . . .
N2 N -0.003(4) 0.746(4) 0.6833(9) Uani 0.15(2) 8 1 d . . .
C1 C 0.542(3) -0.249(4) 0.5330(9) Uani 0.110(13) 8 1 d . . .
C2 C 0.004(4) 0.713(4) 0.6517(9) Uani 0.15(2) 8 1 d . . .
C3 C 1.0210(9) 0.2582(15) 0.3533(5) Uani 0.066(4) 8 1 d . . .
C4 C 1.0903(15) 0.234(2) 0.3262(5) Uani 0.066(4) 8 1 d . . .
C5 C 1.0874(16) 0.243(2) 0.3814(5) Uani 0.066(4) 8 1 d . . .
N3 N 1.031(2) 0.262(2) 0.2988(5) Uani 0.066(4) 8 1 d . . .
N4 N 1.022(2) 0.272(2) 0.4077(5) Uani 0.066(4) 8 1 d . . .
H1n1 H 0.419634 -0.168882 0.517438 Uiso 0.1321 8 1 d . . .
H2n1 H 0.385966 -0.267393 0.529006 Uiso 0.1321 8 1 d . . .
H3n1 H 0.41086 -0.183556 0.548711 Uiso 0.1321 8 1 d . . .
H1n2 H 0.053438 0.782991 0.687748 Uiso 0.1851 8 1 d . . .
H2n2 H -0.061018 0.782795 0.685954 Uiso 0.1851 8 1 d . . .
H3n2 H -0.005222 0.690284 0.694629 Uiso 0.1851 8 1 d . . .
H1c1 H 0.549046 -0.312901 0.522034 Uiso 0.1321 8 1 d . . .
H2c1 H 0.587015 -0.195803 0.524415 Uiso 0.1321 8 1 d . . .
H3c1 H 0.562283 -0.260205 0.553375 Uiso 0.1321 8 1 d . . .
H1c2 H -0.047211 0.657033 0.648141 Uiso 0.1851 8 1 d . . .
H2c2 H -0.013033 0.771134 0.639071 Uiso 0.1851 8 1 d . . .
H3c2 H 0.075185 0.688037 0.647466 Uiso 0.1851 8 1 d . . .
H1c3 H 0.995546 0.32939 0.353557 Uiso 0.0793 8 1 d . . .
H1c4 H 1.155915 0.273663 0.327193 Uiso 0.0793 8 1 d . . .
H2c4 H 1.107002 0.160257 0.325878 Uiso 0.0793 8 1 d . . .
H1c5 H 1.109116 0.171246 0.383024 Uiso 0.0793 8 1 d . . .
H2c5 H 1.150341 0.287268 0.380529 Uiso 0.0793 8 1 d . . .
H1n3 H 1.072681 0.297708 0.286993 Uiso 0.0793 8 1 d . . .
H2n3 H 1.009408 0.205225 0.289795 Uiso 0.0793 8 1 d . . .
H3n3 H 0.974725 0.30007 0.303418 Uiso 0.0793 8 1 d . . .
H1n4 H 1.063407 0.298843 0.421375 Uiso 0.0793 8 1 d . . .
H2n4 H 0.973696 0.318817 0.402507 Uiso 0.0793 8 1 d . . .
H3n4 H 0.989556 0.216931 0.414614 Uiso 0.0793 8 1 d . . .


loop_
_jana_atom_site_ADP_C_label
_jana_atom_site_ADP_C_type_symbol
_jana_atom_site_ADP_C_111
_jana_atom_site_ADP_C_112
_jana_atom_site_ADP_C_113
_jana_atom_site_ADP_C_122
_jana_atom_site_ADP_C_123
_jana_atom_site_ADP_C_133
_jana_atom_site_ADP_C_222
_jana_atom_site_ADP_C_223
_jana_atom_site_ADP_C_233
_jana_atom_site_ADP_C_333
? ? ? ? ? ? ? ? ? ? ? ?

loop_
_jana_atom_site_ADP_D_label
_jana_atom_site_ADP_D_type_symbol
_jana_atom_site_ADP_D_1111
_jana_atom_site_ADP_D_1112
_jana_atom_site_ADP_D_1113
_jana_atom_site_ADP_D_1122
_jana_atom_site_ADP_D_1123
_jana_atom_site_ADP_D_1133
_jana_atom_site_ADP_D_1222
_jana_atom_site_ADP_D_1223
_jana_atom_site_ADP_D_1233
_jana_atom_site_ADP_D_1333
_jana_atom_site_ADP_D_2222
_jana_atom_site_ADP_D_2223
_jana_atom_site_ADP_D_2233
_jana_atom_site_ADP_D_2333
_jana_atom_site_ADP_D_3333
? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ?

loop_
_jana_atom_site_ADP_E_label
_jana_atom_site_ADP_E_type_symbol
_jana_atom_site_ADP_E_11111
_jana_atom_site_ADP_E_11112
_jana_atom_site_ADP_E_11113
_jana_atom_site_ADP_E_11122
_jana_atom_site_ADP_E_11123
_jana_atom_site_ADP_E_11133
_jana_atom_site_ADP_E_11222
_jana_atom_site_ADP_E_11223
_jana_atom_site_ADP_E_11233
_jana_atom_site_ADP_E_11333
_jana_atom_site_ADP_E_12222
_jana_atom_site_ADP_E_12223
_jana_atom_site_ADP_E_12233
_jana_atom_site_ADP_E_12333
_jana_atom_site_ADP_E_13333
_jana_atom_site_ADP_E_22222
_jana_atom_site_ADP_E_22223
_jana_atom_site_ADP_E_22233
_jana_atom_site_ADP_E_22333
_jana_atom_site_ADP_E_23333
_jana_atom_site_ADP_E_33333
? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ?

loop_
_jana_atom_site_ADP_F_label
_jana_atom_site_ADP_F_type_symbol
_jana_atom_site_ADP_F_111111
_jana_atom_site_ADP_F_111112
_jana_atom_site_ADP_F_111113
_jana_atom_site_ADP_F_111122
_jana_atom_site_ADP_F_111123
_jana_atom_site_ADP_F_111133
_jana_atom_site_ADP_F_111222
_jana_atom_site_ADP_F_111223
_jana_atom_site_ADP_F_111233
_jana_atom_site_ADP_F_111333
_jana_atom_site_ADP_F_112222
_jana_atom_site_ADP_F_112223
_jana_atom_site_ADP_F_112233
_jana_atom_site_ADP_F_112333
_jana_atom_site_ADP_F_113333
_jana_atom_site_ADP_F_122222
_jana_atom_site_ADP_F_122223
_jana_atom_site_ADP_F_122233
_jana_atom_site_ADP_F_122333
_jana_atom_site_ADP_F_123333
_jana_atom_site_ADP_F_133333
_jana_atom_site_ADP_F_222222
_jana_atom_site_ADP_F_222223
_jana_atom_site_ADP_F_222233
_jana_atom_site_ADP_F_222333
_jana_atom_site_ADP_F_223333
_jana_atom_site_ADP_F_233333
_jana_atom_site_ADP_F_333333
? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ?


#=======================================================================

# 10. MOLECULAR GEOMETRY


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
I1 Pb1 . 5_544 3.182(2) ?
I1 Pb1 . 6_654 3.182(2) ?
I1 N2 . 3_564 3.74(5) ?
I1 N2 . 4_544 3.74(5) ?
I2 Pb3 . 7_455 3.243(3) ?
I2 Pb3 . 8_545 3.243(3) ?
I2 N4 . 1_455 3.76(3) ?
I2 N4 . 2_655 3.76(3) ?
I3 Pb2 . 5_544 3.154(3) ?
I3 Pb2 . 6_554 3.154(3) ?
I3 N1 . 3_454 3.80(4) ?
I3 N1 . 4_554 3.80(4) ?
Pb1 I5 . . 3.039(4) ?
Pb1 I7 . . 3.337(4) ?
Pb1 I8 . 6_655 3.174(4) ?
Pb1 I8 . 3_465 3.196(4) ?
Pb1 I13 . . 3.242(2) ?
Pb2 I4 . 2_665 3.200(5) ?
Pb2 I7 . . 3.150(5) ?
Pb2 I10 . 5_555 3.1764(13) ?
Pb2 I10 . 4_555 3.1929(13) ?
Pb2 I12 . 5_555 3.177(3) ?
Pb3 I4 . . 3.269(4) ?
Pb3 I6 . 7_555 3.069(4) ?
Pb3 I11 . . 3.187(4) ?
Pb3 I11 . 8_655 3.182(4) ?
Pb3 I14 . 7_555 3.184(2) ?
I4 N1 . 2_655 3.89(4) ?
I4 N1 . 7_555 3.97(3) ?
I5 N3 . 3_465 3.76(3) ?
I5 N3 . 4_655 3.82(3) ?
I6 N4 . 7_455 3.63(3) ?
I6 N4 . 8_645 3.82(3) ?
I7 N2 . . 4.02(5) ?
I7 N2 . 2_565 4.10(5) ?
I8 N2 . 5_644 4.10(5) ?
I8 N2 . 3_564 4.16(5) ?
I8 N3 . 7_455 3.67(2) ?
I9 C3 . . 2.220(15) ?
I9 N3 . . 3.32(2) ?
I9 N4 . . 3.46(2) ?
I10 N1 . 5_554 3.86(3) ?
I11 N1 . 2_655 3.95(3) ?
I11 N4 . . 4.12(2) ?
I11 N4 . 7_455 3.65(2) ?
I13 N3 . 5_455 3.74(3) ?
I13 N3 . 6_655 3.74(3) ?
I14 N1 . . 3.77(3) ?
I14 N1 . 2_655 3.77(3) ?
N1 C1 . . 1.48(5) ?
N1 H1n1 . . 0.87(3) ?
N1 H2n1 . . 0.87(3) ?
N1 H3n1 . . 0.87(3) ?
N2 C2 . . 1.48(6) ?
N2 H1n2 . . 0.87(5) ?
N2 H2n2 . . 0.87(5) ?
N2 H3n2 . . 0.87(5) ?
C1 H1c1 . . 0.96(5) ?
C1 H2c1 . . 0.96(5) ?
C1 H3c1 . . 0.96(4) ?
C2 H1c2 . . 0.97(5) ?
C2 H2c2 . . 0.96(5) ?
C2 H3c2 . . 0.96(5) ?
C3 C4 . . 1.52(3) ?
C3 C5 . . 1.52(3) ?
C3 H1c3 . . 0.960(18) ?
C4 N3 . . 1.48(3) ?
C4 H1c4 . . 0.96(2) ?
C4 H2c4 . . 0.96(3) ?
C5 N4 . . 1.48(3) ?
C5 H1c5 . . 0.96(3) ?
C5 H2c5 . . 0.96(2) ?
N3 H1n3 . . 0.87(2) ?
N3 H2n3 . . 0.87(2) ?
N3 H3n3 . . 0.87(2) ?
N4 H1n4 . . 0.87(2) ?
N4 H2n4 . . 0.88(2) ?
N4 H3n4 . . 0.87(2) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Pb1 I1 Pb1 5_544 . 6_654 150.61(18) ?
Pb1 I1 N2 5_544 . 3_564 94.7(8) ?
Pb1 I1 N2 5_544 . 4_544 99.9(8) ?
Pb1 I1 N2 6_654 . 3_564 99.9(8) ?
Pb1 I1 N2 6_654 . 4_544 94.7(8) ?
N2 I1 N2 3_564 . 4_544 119.9(9) ?
Pb3 I2 Pb3 7_455 . 8_545 148.4(2) ?
Pb3 I2 N4 7_455 . 1_455 90.1(4) ?
Pb3 I2 N4 7_455 . 2_655 102.0(4) ?
Pb3 I2 N4 8_545 . 1_455 102.0(4) ?
Pb3 I2 N4 8_545 . 2_655 90.1(4) ?
N4 I2 N4 1_455 . 2_655 135.1(5) ?
Pb2 I3 Pb2 5_544 . 6_554 157.6(2) ?
Pb2 I3 N1 5_544 . 3_454 110.1(4) ?
Pb2 I3 N1 5_544 . 4_554 84.9(4) ?
Pb2 I3 N1 6_554 . 3_454 84.9(4) ?
Pb2 I3 N1 6_554 . 4_554 110.1(4) ?
N1 I3 N1 3_454 . 4_554 98.1(7) ?
I1 Pb1 I5 5_555 . . 87.69(12) ?
I1 Pb1 I7 5_555 . . 85.95(15) ?
I1 Pb1 I8 5_555 . 6_655 88.23(12) ?
I1 Pb1 I8 5_555 . 3_465 92.96(12) ?
I1 Pb1 I13 5_555 . . 175.24(8) ?
I5 Pb1 I7 . . . 173.05(14) ?
I5 Pb1 I8 . . 6_655 92.80(14) ?
I5 Pb1 I8 . . 3_465 85.99(14) ?
I5 Pb1 I13 . . . 91.76(13) ?
I7 Pb1 I8 . . 6_655 89.81(15) ?
I7 Pb1 I8 . . 3_465 91.52(15) ?
I7 Pb1 I13 . . . 94.81(15) ?
I8 Pb1 I8 6_655 . 3_465 178.27(17) ?
I8 Pb1 I13 6_655 . . 87.07(12) ?
I8 Pb1 I13 3_465 . . 91.72(12) ?
I3 Pb2 I4 5_555 . 2_665 89.33(17) ?
I3 Pb2 I7 5_555 . . 90.39(17) ?
I3 Pb2 I10 5_555 . 5_555 91.37(16) ?
I3 Pb2 I10 5_555 . 4_555 89.05(16) ?
I3 Pb2 I12 5_555 . 5_555 177.53(9) ?
I4 Pb2 I7 2_665 . . 178.79(13) ?
I4 Pb2 I10 2_665 . 5_555 89.80(17) ?
I4 Pb2 I10 2_665 . 4_555 91.40(17) ?
I4 Pb2 I12 2_665 . 5_555 91.86(17) ?
I7 Pb2 I10 . . 5_555 89.02(17) ?
I7 Pb2 I10 . . 4_555 89.77(17) ?
I7 Pb2 I12 . . 5_555 88.47(17) ?
I10 Pb2 I10 5_555 . 4_555 178.7(2) ?
I10 Pb2 I12 5_555 . 5_555 90.80(16) ?
I10 Pb2 I12 4_555 . 5_555 88.76(16) ?
I2 Pb3 I4 7_555 . . 95.27(16) ?
I2 Pb3 I6 7_555 . 7_555 90.70(14) ?
I2 Pb3 I11 7_555 . . 91.55(12) ?
I2 Pb3 I11 7_555 . 8_655 87.71(12) ?
I2 Pb3 I14 7_555 . 7_555 175.65(9) ?
I4 Pb3 I6 . . 7_555 173.08(14) ?
I4 Pb3 I11 . . . 90.22(15) ?
I4 Pb3 I11 . . 8_655 89.83(15) ?
I4 Pb3 I14 . . 7_555 85.91(15) ?
I6 Pb3 I11 7_555 . . 86.10(14) ?
I6 Pb3 I11 7_555 . 8_655 93.91(14) ?
I6 Pb3 I14 7_555 . 7_555 88.40(12) ?
I11 Pb3 I11 . . 8_655 179.26(17) ?
I11 Pb3 I14 . . 7_555 92.63(12) ?
I11 Pb3 I14 8_655 . 7_555 88.11(12) ?
Pb2 I4 Pb3 2_665 . . 158.9(2) ?
Pb2 I4 N1 2_665 . 2_655 94.5(5) ?
Pb2 I4 N1 2_665 . 7_555 81.5(5) ?
Pb3 I4 N1 . . 2_655 94.8(5) ?
Pb3 I4 N1 . . 7_555 83.4(5) ?
N1 I4 N1 2_655 . 7_555 160.1(6) ?
Pb1 I5 N3 . . 3_465 98.3(4) ?
Pb1 I5 N3 . . 4_655 89.4(4) ?
N3 I5 N3 3_465 . 4_655 107.6(5) ?
Pb3 I6 N4 7_455 . 7_455 94.5(4) ?
Pb3 I6 N4 7_455 . 8_645 86.0(4) ?
N4 I6 N4 7_455 . 8_645 103.0(6) ?
Pb1 I7 Pb2 . . . 158.5(2) ?
Pb1 I7 N2 . . . 87.7(6) ?
Pb1 I7 N2 . . 2_565 88.8(6) ?
Pb2 I7 N2 . . . 105.7(6) ?
Pb2 I7 N2 . . 2_565 104.6(6) ?
N2 I7 N2 . . 2_565 101.2(10) ?
Pb1 I8 Pb1 6_654 . 3_564 178.5(2) ?
Pb1 I8 N2 6_654 . 5_644 91.1(7) ?
Pb1 I8 N2 6_654 . 3_564 91.9(7) ?
Pb1 I8 N3 6_654 . 7_455 90.0(4) ?
Pb1 I8 N2 3_564 . 5_644 87.9(7) ?
Pb1 I8 N2 3_564 . 3_564 87.1(7) ?
Pb1 I8 N3 3_564 . 7_455 91.0(4) ?
N2 I8 N2 5_644 . 3_564 97.4(9) ?
N2 I8 N3 5_644 . 7_455 178.7(8) ?
N2 I8 N3 3_564 . 7_455 83.2(7) ?
C3 I9 N3 . . . 47.7(7) ?
C3 I9 N4 . . . 44.8(7) ?
N3 I9 N4 . . . 92.5(6) ?
Pb2 I10 Pb2 5_544 . 4_554 178.7(3) ?
Pb2 I10 N1 5_544 . 5_554 95.6(6) ?
Pb2 I10 N1 4_554 . 5_554 83.4(6) ?
Pb3 I11 Pb3 . . 8_645 179.6(2) ?
Pb3 I11 N1 . . 2_655 95.1(6) ?
Pb3 I11 N4 . . . 84.1(4) ?
Pb3 I11 N4 . . 7_455 93.0(4) ?
Pb3 I11 N1 8_645 . 2_655 84.9(6) ?
Pb3 I11 N4 8_645 . . 95.8(4) ?
Pb3 I11 N4 8_645 . 7_455 87.4(4) ?
N1 I11 N4 2_655 . . 158.5(5) ?
N1 I11 N4 2_655 . 7_455 95.2(6) ?
N4 I11 N4 . . 7_455 106.3(5) ?
Pb2 I12 Pb2 5_544 . 6_654 155.3(2) ?
Pb1 I13 Pb1 . . 2_565 148.9(2) ?
Pb1 I13 N3 . . 5_455 89.0(4) ?
Pb1 I13 N3 . . 6_655 104.6(4) ?
Pb1 I13 N3 2_565 . 5_455 104.6(4) ?
Pb1 I13 N3 2_565 . 6_655 89.0(4) ?
N3 I13 N3 5_455 . 6_655 128.0(5) ?
Pb3 I14 Pb3 7_455 . 8_645 150.75(18) ?
Pb3 I14 N1 7_455 . . 87.8(4) ?
Pb3 I14 N1 7_455 . 2_655 111.5(4) ?
Pb3 I14 N1 8_645 . . 111.5(4) ?
Pb3 I14 N1 8_645 . 2_655 87.8(4) ?
N1 I14 N1 . . 2_655 98.9(7) ?
I3 N1 I4 3_555 . 2_655 139.2(9) ?
I3 N1 I4 3_555 . 7_455 70.1(6) ?
I3 N1 I10 3_555 . 5_545 71.1(6) ?
I3 N1 I11 3_555 . 2_655 137.2(10) ?
I3 N1 I14 3_555 . . 81.5(7) ?
I3 N1 C1 3_555 . . 88(2) ?
I3 N1 H1n1 3_555 . . 92(2) ?
I3 N1 H2n1 3_555 . . 143(2) ?
I3 N1 H3n1 3_555 . . 34.2(17) ?
I4 N1 I4 2_655 . 7_455 110.8(6) ?
I4 N1 I10 2_655 . 5_545 71.0(6) ?
I4 N1 I11 2_655 . 2_655 71.4(6) ?
I4 N1 I14 2_655 . . 138.4(9) ?
I4 N1 C1 2_655 . . 97(3) ?
I4 N1 H1n1 2_655 . . 123(2) ?
I4 N1 H2n1 2_655 . . 15.0(17) ?
I4 N1 H3n1 2_655 . . 108(2) ?
I4 N1 I10 7_455 . 5_545 71.5(5) ?
I4 N1 I11 7_455 . 2_655 70.2(5) ?
I4 N1 I14 7_455 . . 69.1(6) ?
I4 N1 C1 7_455 . . 152(3) ?
I4 N1 H1n1 7_455 . . 55.9(18) ?
I4 N1 H2n1 7_455 . . 97.8(19) ?
I4 N1 H3n1 7_455 . . 61.5(19) ?
I10 N1 I11 5_545 . 2_655 110.2(6) ?
I10 N1 I14 5_545 . . 137.8(10) ?
I10 N1 C1 5_545 . . 119(2) ?
I10 N1 H1n1 5_545 . . 127(2) ?
I10 N1 H2n1 5_545 . . 72.3(19) ?
I10 N1 H3n1 5_545 . . 37.4(18) ?
I11 N1 I14 2_655 . . 69.9(6) ?
I11 N1 C1 2_655 . . 122(2) ?
I11 N1 H1n1 2_655 . . 51.4(18) ?
I11 N1 H2n1 2_655 . . 58.3(18) ?
I11 N1 H3n1 2_655 . . 128(2) ?
I14 N1 C1 . . . 91(2) ?
I14 N1 H1n1 . . . 21.5(14) ?
I14 N1 H2n1 . . . 128(2) ?
I14 N1 H3n1 . . . 107(3) ?
C1 N1 H1n1 . . . 110(3) ?
C1 N1 H2n1 . . . 110(4) ?
C1 N1 H3n1 . . . 110(3) ?
H1n1 N1 H2n1 . . . 109(3) ?
H1n1 N1 H3n1 . . . 109(4) ?
H2n1 N1 H3n1 . . . 109(3) ?
I1 N2 I7 3_465 . . 136.6(13) ?
I1 N2 I7 3_465 . 2_565 139.4(13) ?
I1 N2 I8 3_465 . 5_455 72.2(8) ?
I1 N2 I8 3_465 . 3_465 67.9(7) ?
I1 N2 C2 3_465 . . 136(3) ?
I1 N2 H1n2 3_465 . . 54(3) ?
I1 N2 H2n2 3_465 . . 58(3) ?
I1 N2 H3n2 3_465 . . 114(3) ?
I7 N2 I7 . . 2_565 76.2(9) ?
I7 N2 I8 . . 5_455 123.7(12) ?
I7 N2 I8 . . 3_465 69.9(8) ?
I7 N2 C2 . . . 67(3) ?
I7 N2 H1n2 . . . 86(3) ?
I7 N2 H2n2 . . . 163(4) ?
I7 N2 H3n2 . . . 59(3) ?
I7 N2 I8 2_565 . 5_455 68.3(8) ?
I7 N2 I8 2_565 . 3_465 125.9(12) ?
I7 N2 C2 2_565 . . 71(3) ?
I7 N2 H1n2 2_565 . . 161(4) ?
I7 N2 H2n2 2_565 . . 87(3) ?
I7 N2 H3n2 2_565 . . 55(3) ?
I8 N2 I8 5_455 . 3_465 97.5(9) ?
I8 N2 C2 5_455 . . 132(3) ?
I8 N2 H1n2 5_455 . . 118(3) ?
I8 N2 H2n2 5_455 . . 46(3) ?
I8 N2 H3n2 5_455 . . 65(3) ?
I8 N2 C2 3_465 . . 127(3) ?
I8 N2 H1n2 3_465 . . 38(2) ?
I8 N2 H2n2 3_465 . . 121(3) ?
I8 N2 H3n2 3_465 . . 71(3) ?
C2 N2 H1n2 . . . 109(4) ?
C2 N2 H2n2 . . . 109(4) ?
C2 N2 H3n2 . . . 109(5) ?
H1n2 N2 H2n2 . . . 110(5) ?
H1n2 N2 H3n2 . . . 109(5) ?
H2n2 N2 H3n2 . . . 109(5) ?
N1 C1 H1c1 . . . 109(4) ?
N1 C1 H2c1 . . . 109(4) ?
N1 C1 H3c1 . . . 109(3) ?
H1c1 C1 H2c1 . . . 110(4) ?
H1c1 C1 H3c1 . . . 110(5) ?
H2c1 C1 H3c1 . . . 110(4) ?
N2 C2 H1c2 . . . 109(4) ?
N2 C2 H2c2 . . . 110(4) ?
N2 C2 H3c2 . . . 110(4) ?
H1c2 C2 H2c2 . . . 109(4) ?
H1c2 C2 H3c2 . . . 109(5) ?
H2c2 C2 H3c2 . . . 110(4) ?
I9 C3 C4 . . . 105.7(13) ?
I9 C3 C5 . . . 112.1(14) ?
I9 C3 H1c3 . . . 110.2(8) ?
C4 C3 C5 . . . 109.4(13) ?
C4 C3 H1c3 . . . 112.7(19) ?
C5 C3 H1c3 . . . 106.8(19) ?
C3 C4 N3 . . . 109.7(17) ?
C3 C4 H1c4 . . . 110(2) ?
C3 C4 H2c4 . . . 109(2) ?
N3 C4 H1c4 . . . 109(2) ?
N3 C4 H2c4 . . . 109(2) ?
H1c4 C4 H2c4 . . . 109.4(19) ?
C3 C5 N4 . . . 109.5(17) ?
C3 C5 H1c5 . . . 110(2) ?
C3 C5 H2c5 . . . 109(2) ?
N4 C5 H1c5 . . . 109(2) ?
N4 C5 H2c5 . . . 109(2) ?
H1c5 C5 H2c5 . . . 110(2) ?
I5 N3 I5 3_564 . 4_654 71.1(5) ?
I5 N3 I8 3_564 . 7_555 125.2(7) ?
I5 N3 I9 3_564 . . 82.3(5) ?
I5 N3 I13 3_564 . 5_644 128.4(7) ?
I5 N3 C4 3_564 . . 115.3(14) ?
I5 N3 H1n3 3_564 . . 95.2(17) ?
I5 N3 H2n3 3_564 . . 116.1(18) ?
I5 N3 H3n3 3_564 . . 14.0(13) ?
I5 N3 I8 4_654 . 7_555 73.9(5) ?
I5 N3 I9 4_654 . . 125.0(7) ?
I5 N3 I13 4_654 . 5_644 151.1(7) ?
I5 N3 C4 4_654 . . 83.8(14) ?
I5 N3 H1n3 4_654 . . 47.5(14) ?
I5 N3 H2n3 4_654 . . 156.9(18) ?
I5 N3 H3n3 4_654 . . 82.2(17) ?
I8 N3 I9 7_555 . . 152.2(8) ?
I8 N3 I13 7_555 . 5_644 77.2(5) ?
I8 N3 C4 7_555 . . 101.0(13) ?
I8 N3 H1n3 7_555 . . 31.9(13) ?
I8 N3 H2n3 7_555 . . 85.0(16) ?
I8 N3 H3n3 7_555 . . 138.7(19) ?
I9 N3 I13 . . 5_644 82.0(6) ?
I9 N3 C4 . . . 65.2(12) ?
I9 N3 H1n3 . . . 172(2) ?
I9 N3 H2n3 . . . 78.1(15) ?
I9 N3 H3n3 . . . 68.5(15) ?
I13 N3 C4 5_644 . . 101.6(15) ?
I13 N3 H1n3 5_644 . . 105.1(17) ?
I13 N3 H2n3 5_644 . . 12.4(13) ?
I13 N3 H3n3 5_644 . . 121.1(19) ?
C4 N3 H1n3 . . . 110(2) ?
C4 N3 H2n3 . . . 110(2) ?
C4 N3 H3n3 . . . 109(2) ?
H1n3 N3 H2n3 . . . 110(2) ?
H1n3 N3 H3n3 . . . 109(3) ?
H2n3 N3 H3n3 . . . 109(3) ?
I2 N4 I6 1_655 . 7_555 131.9(7) ?
I2 N4 I6 1_655 . 8_655 151.4(7) ?
I2 N4 I9 1_655 . . 79.8(5) ?
I2 N4 I11 1_655 . . 68.7(4) ?
I2 N4 I11 1_655 . 7_555 76.9(5) ?
I2 N4 C5 1_655 . . 96.6(15) ?
I2 N4 H1n4 1_655 . . 97.8(17) ?
I2 N4 H2n4 1_655 . . 132.8(19) ?
I2 N4 H3n4 1_655 . . 23.5(13) ?
I6 N4 I6 7_555 . 8_655 73.8(5) ?
I6 N4 I9 7_555 . . 81.8(5) ?
I6 N4 I11 7_555 . . 66.6(4) ?
I6 N4 I11 7_555 . 7_555 131.9(7) ?
I6 N4 C5 7_555 . . 114.6(14) ?
I6 N4 H1n4 7_555 . . 104.2(18) ?
I6 N4 H2n4 7_555 . . 5.7(11) ?
I6 N4 H3n4 7_555 . . 108.5(18) ?
I6 N4 I9 8_655 . . 121.5(6) ?
I6 N4 I11 8_655 . . 126.2(6) ?
I6 N4 I11 8_655 . 7_555 75.4(5) ?
I6 N4 C5 8_655 . . 78.7(14) ?
I6 N4 H1n4 8_655 . . 58.8(15) ?
I6 N4 H2n4 8_655 . . 74.2(16) ?
I6 N4 H3n4 8_655 . . 168.2(18) ?
I9 N4 I11 . . . 87.7(5) ?
I9 N4 I11 . . 7_555 146.3(8) ?
I9 N4 C5 . . . 64.6(12) ?
I9 N4 H1n4 . . . 173(2) ?
I9 N4 H2n4 . . . 77.0(15) ?
I9 N4 H3n4 . . . 70.2(15) ?
I11 N4 I11 . . 7_555 105.8(5) ?
I11 N4 C5 . . . 151.0(15) ?
I11 N4 H1n4 . . . 97.2(16) ?
I11 N4 H2n4 . . . 69.8(15) ?
I11 N4 H3n4 . . . 48.6(14) ?
I11 N4 C5 7_555 . . 94.2(13) ?
I11 N4 H1n4 7_555 . . 27.7(13) ?
I11 N4 H2n4 7_555 . . 136.5(19) ?
I11 N4 H3n4 7_555 . . 95.5(16) ?
C5 N4 H1n4 . . . 110(2) ?
C5 N4 H2n4 . . . 109(2) ?
C5 N4 H3n4 . . . 110(2) ?
H1n4 N4 H2n4 . . . 109(3) ?
H1n4 N4 H3n4 . . . 110(2) ?
H2n4 N4 H3n4 . . . 109(3) ?

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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
? ? ? ? ? ? ? ? ? ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
? ? ? ? ? ? ? ? ? ? ?


#=======================================================================

# 11. STRUCTURE-FACTOR LIST



####################################################################### 
# 
# 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_n=4_(DicI)(MA)3Pb4I13
_database_code_depnum_ccdc_archive 'CCDC 2283265'
loop_
_audit_author_name
_audit_author_address
'Nicolas Mercier'
;UNIV Angers, UMR CNRS
France
;
_audit_update_record             
;
2023-11-24 deposited with the CCDC.	2023-11-30 downloaded from the CCDC.
;
#=======================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic        
; ?
;
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_iupac          ?
_chemical_formula_sum            'C6 H29 I14 N5 Pb4'
_chemical_formula_weight         2776.8
_chemical_melting_point          ?
_chemical_compound_source        ?
_chemical_absolute_configuration ?

#=======================================================================

# 6. CRYSTAL DATA

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b a 2'
_symmetry_space_group_name_Hall  'P -2xab;-2yab;2z'
_symmetry_Int_Tables_number      32

loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,-y,z
3 x+1/2,-y+1/2,z
4 -x+1/2,y+1/2,z

_cell_length_a                   12.4176(5)
_cell_length_b                   12.7217(5)
_cell_length_c                   28.7245(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4537.7(3)

loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.53(4) 1 0 0 0 1 0 0 0 1
2 0.47(4) -1 0 0 0 -1 0 0 0 -1

_cell_formula_units_Z            4

_cell_measurement_reflns_used    8111
_cell_measurement_theta_min      3
_cell_measurement_theta_max      75.96
_cell_measurement_temperature    293
_cell_special_details            
; ?
;

_exptl_crystal_density_diffrn    4.0646
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             4680

_exptl_absorpt_coefficient_mu    103.173
_exptl_crystal_description       'square platelets'
_exptl_crystal_size_max          0.103
_exptl_crystal_size_mid          0.066
_exptl_crystal_size_min          0.020
_exptl_crystal_size_rad          ?
_exptl_crystal_colour            black
_exptl_absorpt_correction_type   multi-scan
_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_absorpt_correction_T_min  0.063
_exptl_absorpt_correction_T_max  1
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
? ? ? ?

#=======================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           ?


_diffrn_ambient_temperature      293
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_power             ?
_diffrn_source_voltage           ?
_diffrn_source_current           ?
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'SuperNova, Single source at offset/far, AtlasS2'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1990
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support ?


_diffrn_reflns_number            49382
_diffrn_reflns_theta_min         3.08
_diffrn_reflns_theta_max         76.38
_diffrn_reflns_theta_full        76.38
_diffrn_measured_fraction_theta_max 1
_diffrn_measured_fraction_theta_full 1
_diffrn_reflns_av_R_equivalents  0.0784
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_reduction_process ?

_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?

_diffrn_radiation_probe          X-ray

#=======================================================================

# 8. REFINEMENT DATA

_refine_special_details          
; ?
;

_reflns_number_total             8004
_reflns_number_gt                5337
_reflns_threshold_expression     I>2σ(I)

_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_gt           0.0471
_refine_ls_wR_factor_gt          0.0966
_refine_ls_R_factor_all          0.0739
_refine_ls_wR_factor_ref         0.1038
_refine_ls_goodness_of_fit_ref   1.33
_refine_ls_goodness_of_fit_gt    1.53
_refine_ls_restrained_S_gt       ?
_refine_ls_restrained_S_all      ?
_refine_ls_number_reflns         8004
_refine_ls_number_parameters     212
_refine_ls_number_restraints     7
_refine_ls_number_constraints    117
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     w=1/(σ²(I)+0.0004I²)
_refine_ls_hydrogen_treatment    constr
_refine_ls_shift/su_max          0.0468
_refine_ls_shift/su_mean         0.0059
_refine_diff_density_max         2.15
_refine_diff_density_min         -2.25
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_extinction_expression ?
_refine_ls_abs_structure_details 
;  3799 of Friedel pairs used in the refinement
;
_refine_ls_abs_structure_Flack   0.47(4)
_refine_ls_abs_structure_Rogers  ?

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0.0181 0.0091 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
H 0.0000 0.0000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
I -0.3257 6.8362 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
N 0.0311 0.0180 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
Pb -4.0753 8.5060 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'

_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_structure_solution    'Charge flipping'
_computing_structure_refinement  Jana2006
_computing_molecular_graphics    ?
_computing_publication_material  ?

loop_
_restr_distance_atom_site_label_1
_restr_distance_site_symmetry_1
_restr_distance_atom_site_label_2
_restr_distance_site_symmetry_2
_restr_distance_target
_restr_distance_target_weight_param
C1 . N1 . 1.48 0.001
C2 . N2 . 1.48 0.001
N3 . C6 . 1.48 0.001
C4 . N4 . 1.48 0.001
C5 . N5 . 1.48 0.001
C5 . C3 . 1.52 0.001
C3 . C4 . 1.52 0.001


#=======================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_adp_type
_atom_site_U_iso_or_equiv
_atom_site_site_symmetry_multiplicity
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.74961(14) 0.4972(2) 0.186435(3) Uani 0.0291(5) 4 1 d . . .
Pb2 Pb 0.25159(15) 0.00944(16) 0.965189(3) Uani 0.0312(6) 4 1 d . . .
I1 I 0.7504(4) 0.7477(3) 0.186565(8) Uani 0.0634(15) 4 1 d . . .
I2 I 0 0 0.206719(8) Uani 0.075(2) 2 1 d . . .
I3 I 0.2040(4) 0.0055(5) 0.514273(8) Uani 0.0666(14) 4 1 d . . .
I4 I 0 0 0.935163(8) Uani 0.0569(17) 2 1 d . . .
I5 I 0.2499(4) 0.2601(3) 0.963927(8) Uani 0.0582(13) 4 1 d . . .
I6 I 0.5 0 0.164110(8) Uani 0.0611(14) 2 1 d . . .
I7 I 0.5 0 0.992627(8) Uani 0.065(2) 2 1 d . . .
I8 I 0.8230(3) 0.4746(3) 0.728864(8) Uani 0.0517(12) 4 1 d . . .
I9 I 0.3219(3) 0.0228(3) 0.863918(8) Uani 0.0524(12) 4 1 d . . .
I10 I 0.29373(12) 0.00240(12) 0.297355(8) Uani 0.0657(4) 4 1 d . . .
I11 I 0.2026(4) 0.0054(5) 0.079143(8) Uani 0.0681(15) 4 1 d . . .
Pb3 Pb 0.75253(15) 0.49154(17) 0.627377(3) Uani 0.0318(6) 4 1 d . . .
I12 I 0.61785(12) 0.64883(11) 0.795817(8) Uani 0.0770(5) 4 1 d . . .
Pb4 Pb 0.74939(14) 0.4977(2) 0.406520(3) Uani 0.0301(5) 4 1 d . . .
I13 I 0.5 0 0.599135(8) Uani 0.064(2) 2 1 d . . .
I14 I 0 0 0.657178(8) Uani 0.0570(17) 2 1 d . . .
I15 I 1 0.5 0.425152(8) Uani 0.0795(19) 2 1 d . . .
I16 I 0 0 0.383721(8) Uani 0.0620(16) 2 1 d . . .
I17 I 0.7493(5) 0.2478(4) 0.405330(8) Uani 0.0652(16) 4 1 d . . .
I18 I 0.7493(4) 0.2410(3) 0.627771(8) Uani 0.0685(16) 4 1 d . . .
N1 N 0.5018(2) -0.26266(18) 0.53500(6) Uiso 0.149(14) 4 1 d . . .
N2 N 0.06510(15) 0.28199(18) 0.07976(9) Uiso 0.115(10) 4 1 d . . .
N3 N -0.03248(15) -0.25587(18) 0.27751(9) Uiso 0.167(15) 4 1 d . . .
C1 C 0.5034(2) -0.2879(2) 0.48471(6) Uiso 0.083(9) 4 1 d . . .
C2 C -0.05301(15) 0.26668(19) 0.07822(9) Uiso 0.098(10) 4 1 d . . .
C3 C 0.4864(3) 0.7617(4) 0.79434(12) Uiso 0.045(4) 4 1 d . . .
C4 C 0.4189(3) 0.7442(2) 0.75089(7) Uiso 0.035(4) 4 1 d . . .
N4 N 0.48188(19) 0.7689(2) 0.70851(7) Uiso 0.026(3) 4 1 d . . .
C5 C 0.4006(3) 0.7198(2) 0.82716(7) Uiso 0.113(12) 4 1 d . . .
N5 N 0.4571(2) 0.75584(19) 0.86963(7) Uiso 0.163(14) 4 1 d . . .
C6 C 0.05598(16) -0.24119(19) 0.31141(9) Uiso 0.21(2) 4 1 d . . .
H1n1 H 0.483279 -0.318282 0.550699 Uiso 0.1793 4 1 d . . .
H2n1 H 0.565528 -0.242273 0.543716 Uiso 0.1793 4 1 d . . .
H3n1 H 0.455543 -0.212594 0.540141 Uiso 0.1793 4 1 d . . .
H1n2 H 0.081724 0.34026 0.065622 Uiso 0.1378 4 1 d . . .
H2n2 H 0.086218 0.285169 0.108601 Uiso 0.1378 4 1 d . . .
H3n2 H 0.096766 0.229556 0.065953 Uiso 0.1378 4 1 d . . .
H1n3 H -0.020767 -0.312437 0.261261 Uiso 0.2009 4 1 d . . .
H2n3 H -0.093256 -0.261999 0.292329 Uiso 0.2009 4 1 d . . .
H3n3 H -0.035421 -0.201798 0.259008 Uiso 0.2009 4 1 d . . .
H1c1 H 0.431178 -0.300243 0.474085 Uiso 0.0994 4 1 d . . .
H2c1 H 0.533884 -0.230008 0.467791 Uiso 0.0994 4 1 d . . .
H3c1 H 0.546092 -0.349708 0.479635 Uiso 0.0994 4 1 d . . .
H1c2 H -0.087836 0.333489 0.074366 Uiso 0.1182 4 1 d . . .
H2c2 H -0.071103 0.221737 0.052534 Uiso 0.1182 4 1 d . . .
H3c2 H -0.076681 0.23489 0.106744 Uiso 0.1182 4 1 d . . .
H1c3 H 0.516844 0.830254 0.799089 Uiso 0.0534 4 1 d . . .
H1c4 H 0.39561 0.67233 0.749759 Uiso 0.0418 4 1 d . . .
H2c4 H 0.356197 0.788298 0.752048 Uiso 0.0418 4 1 d . . .
H1n4 H 0.440301 0.764708 0.684201 Uiso 0.0312 4 1 d . . .
H2n4 H 0.507809 0.832244 0.710657 Uiso 0.0312 4 1 d . . .
H3n4 H 0.534553 0.724227 0.705757 Uiso 0.0312 4 1 d . . .
H1c5 H 0.335449 0.75945 0.823237 Uiso 0.1351 4 1 d . . .
H2c5 H 0.400581 0.644343 0.826206 Uiso 0.1351 4 1 d . . .
H1n5 H 0.520806 0.778895 0.862195 Uiso 0.1954 4 1 d . . .
H2n5 H 0.420431 0.806163 0.882628 Uiso 0.1954 4 1 d . . .
H3n5 H 0.46337 0.703662 0.889019 Uiso 0.1954 4 1 d . . .
H1c6 H 0.070114 -0.306498 0.326992 Uiso 0.2551 4 1 d . . .
H2c6 H 0.119682 -0.218532 0.295344 Uiso 0.2551 4 1 d . . .
H3c6 H 0.03554 -0.189003 0.333872 Uiso 0.2551 4 1 d . . .


loop_
_jana_atom_site_ADP_C_label
_jana_atom_site_ADP_C_type_symbol
_jana_atom_site_ADP_C_111
_jana_atom_site_ADP_C_112
_jana_atom_site_ADP_C_113
_jana_atom_site_ADP_C_122
_jana_atom_site_ADP_C_123
_jana_atom_site_ADP_C_133
_jana_atom_site_ADP_C_222
_jana_atom_site_ADP_C_223
_jana_atom_site_ADP_C_233
_jana_atom_site_ADP_C_333
? ? ? ? ? ? ? ? ? ? ? ?

loop_
_jana_atom_site_ADP_D_label
_jana_atom_site_ADP_D_type_symbol
_jana_atom_site_ADP_D_1111
_jana_atom_site_ADP_D_1112
_jana_atom_site_ADP_D_1113
_jana_atom_site_ADP_D_1122
_jana_atom_site_ADP_D_1123
_jana_atom_site_ADP_D_1133
_jana_atom_site_ADP_D_1222
_jana_atom_site_ADP_D_1223
_jana_atom_site_ADP_D_1233
_jana_atom_site_ADP_D_1333
_jana_atom_site_ADP_D_2222
_jana_atom_site_ADP_D_2223
_jana_atom_site_ADP_D_2233
_jana_atom_site_ADP_D_2333
_jana_atom_site_ADP_D_3333
? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ?

loop_
_jana_atom_site_ADP_E_label
_jana_atom_site_ADP_E_type_symbol
_jana_atom_site_ADP_E_11111
_jana_atom_site_ADP_E_11112
_jana_atom_site_ADP_E_11113
_jana_atom_site_ADP_E_11122
_jana_atom_site_ADP_E_11123
_jana_atom_site_ADP_E_11133
_jana_atom_site_ADP_E_11222
_jana_atom_site_ADP_E_11223
_jana_atom_site_ADP_E_11233
_jana_atom_site_ADP_E_11333
_jana_atom_site_ADP_E_12222
_jana_atom_site_ADP_E_12223
_jana_atom_site_ADP_E_12233
_jana_atom_site_ADP_E_12333
_jana_atom_site_ADP_E_13333
_jana_atom_site_ADP_E_22222
_jana_atom_site_ADP_E_22223
_jana_atom_site_ADP_E_22233
_jana_atom_site_ADP_E_22333
_jana_atom_site_ADP_E_23333
_jana_atom_site_ADP_E_33333
? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ?

loop_
_jana_atom_site_ADP_F_label
_jana_atom_site_ADP_F_type_symbol
_jana_atom_site_ADP_F_111111
_jana_atom_site_ADP_F_111112
_jana_atom_site_ADP_F_111113
_jana_atom_site_ADP_F_111122
_jana_atom_site_ADP_F_111123
_jana_atom_site_ADP_F_111133
_jana_atom_site_ADP_F_111222
_jana_atom_site_ADP_F_111223
_jana_atom_site_ADP_F_111233
_jana_atom_site_ADP_F_111333
_jana_atom_site_ADP_F_112222
_jana_atom_site_ADP_F_112223
_jana_atom_site_ADP_F_112233
_jana_atom_site_ADP_F_112333
_jana_atom_site_ADP_F_113333
_jana_atom_site_ADP_F_122222
_jana_atom_site_ADP_F_122223
_jana_atom_site_ADP_F_122233
_jana_atom_site_ADP_F_122333
_jana_atom_site_ADP_F_123333
_jana_atom_site_ADP_F_133333
_jana_atom_site_ADP_F_222222
_jana_atom_site_ADP_F_222223
_jana_atom_site_ADP_F_222233
_jana_atom_site_ADP_F_222333
_jana_atom_site_ADP_F_223333
_jana_atom_site_ADP_F_233333
_jana_atom_site_ADP_F_333333
? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ?


#=======================================================================

# 10. MOLECULAR GEOMETRY


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pb1 I1 . . 3.187(5) ?
Pb1 I1 . 4_645 3.174(5) ?
Pb1 I2 . 3_555 3.1540(17) ?
Pb1 I6 . 3_555 3.1749(17) ?
Pb1 I10 . 3_555 3.2329(5) ?
Pb1 I11 . 3_555 3.1369(10) ?
Pb2 I4 . . 3.2432(18) ?
Pb2 I5 . . 3.189(4) ?
Pb2 I5 . 4_545 3.172(4) ?
Pb2 I7 . . 3.1860(18) ?
Pb2 I9 . . 3.0419(13) ?
Pb2 I11 . 1_556 3.3297(10) ?
I1 N2 . 2_665 3.848(4) ?
I1 N3 . 1_665 3.754(4) ?
I2 N3 . . 3.859(2) ?
I2 N3 . 2_555 3.859(2) ?
I3 Pb3 . 3_455 3.3045(10) ?
I3 Pb4 . 3_455 3.1463(10) ?
I3 N1 . 3_445 4.025(6) ?
I3 N1 . 4_555 3.948(6) ?
I4 N5 . 3_455 3.797(2) ?
I4 N5 . 4_545 3.797(2) ?
I5 N2 . 1_556 4.051(4) ?
I5 N5 . 4_545 3.735(4) ?
I6 N2 . 3_555 3.770(2) ?
I6 N2 . 4_545 3.770(2) ?
I7 N2 . 3_556 3.822(2) ?
I7 N2 . 4_546 3.822(2) ?
I8 Pb3 . . 3.0513(13) ?
I8 N4 . 3_565 3.858(5) ?
I8 N4 . 4_645 3.614(4) ?
I9 N5 . 1_545 3.792(5) ?
I9 N5 . 2_665 3.936(5) ?
I10 Pb4 . 3_455 3.1837(5) ?
I10 N3 . 3_545 3.849(3) ?
I11 N2 . . 3.911(7) ?
I11 N2 . 4_545 4.050(6) ?
Pb3 I13 . 3_555 3.1801(18) ?
Pb3 I14 . 3_555 3.2523(18) ?
Pb3 I18 . . 3.188(4) ?
Pb3 I18 . 4_655 3.174(4) ?
I12 C3 . . 2.174(5) ?
I12 N4 . . 3.387(2) ?
I12 N5 . . 3.215(3) ?
Pb4 I15 . . 3.1578(17) ?
Pb4 I16 . 3_555 3.1654(17) ?
Pb4 I17 . . 3.179(6) ?
Pb4 I17 . 4_655 3.182(6) ?
I13 N1 . . 3.816(2) ?
I13 N1 . 2_655 3.816(2) ?
I14 N4 . 3_455 3.732(2) ?
I14 N4 . 4_545 3.732(2) ?
I18 N1 . 2_655 4.111(4) ?
I18 N1 . 4_655 4.081(4) ?
I18 N4 . 2_665 3.693(4) ?
I18 N4 . 4_645 4.080(5) ?
N1 C1 . . 1.480(2) ?
N1 H1n1 . . 0.870(2) ?
N1 H2n1 . . 0.870(2) ?
N1 H3n1 . . 0.870(2) ?
N2 C2 . . 1.480(3) ?
N2 H1n2 . . 0.870(2) ?
N2 H2n2 . . 0.870(3) ?
N2 H3n2 . . 0.870(2) ?
N3 C6 . . 1.480(3) ?
N3 H1n3 . . 0.870(2) ?
N3 H2n3 . . 0.870(2) ?
N3 H3n3 . . 0.870(2) ?
C1 H1c1 . . 0.960(2) ?
C1 H2c1 . . 0.960(2) ?
C1 H3c1 . . 0.959(3) ?
C2 H1c2 . . 0.960(2) ?
C2 H2c2 . . 0.960(2) ?
C2 H3c2 . . 0.960(2) ?
C3 C4 . . 1.520(4) ?
C3 C5 . . 1.519(5) ?
C3 H1c3 . . 0.960(5) ?
C4 N4 . . 1.481(3) ?
C4 H1c4 . . 0.960(3) ?
C4 H2c4 . . 0.960(3) ?
N4 H1n4 . . 0.870(2) ?
N4 H2n4 . . 0.870(3) ?
N4 H3n4 . . 0.870(2) ?
C5 N5 . . 1.480(3) ?
C5 H1c5 . . 0.960(3) ?
C5 H2c5 . . 0.960(3) ?
N5 H1n5 . . 0.870(2) ?
N5 H2n5 . . 0.870(2) ?
N5 H3n5 . . 0.870(2) ?
C6 H1c6 . . 0.960(2) ?
C6 H2c6 . . 0.960(2) ?
C6 H3c6 . . 0.960(2) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
I1 Pb1 I1 . . 4_645 179.78(11) ?
I1 Pb1 I2 . . 3_555 89.51(10) ?
I1 Pb1 I6 . . 3_555 89.20(10) ?
I1 Pb1 I10 . . 3_555 89.81(6) ?
I1 Pb1 I11 . . 3_555 90.70(13) ?
I1 Pb1 I2 4_645 . 3_555 90.63(10) ?
I1 Pb1 I6 4_645 . 3_555 90.66(10) ?
I1 Pb1 I10 4_645 . 3_555 90.02(6) ?
I1 Pb1 I11 4_645 . 3_555 89.46(13) ?
I2 Pb1 I6 3_555 . 3_555 178.36(7) ?
I2 Pb1 I10 3_555 . 3_555 89.11(4) ?
I2 Pb1 I11 3_555 . 3_555 89.93(10) ?
I6 Pb1 I10 3_555 . 3_555 91.90(5) ?
I6 Pb1 I11 3_555 . 3_555 89.08(9) ?
I10 Pb1 I11 3_555 . 3_555 178.90(12) ?
I4 Pb2 I5 . . . 91.59(10) ?
I4 Pb2 I5 . . 4_545 87.38(10) ?
I4 Pb2 I7 . . . 175.58(7) ?
I4 Pb2 I9 . . . 91.39(7) ?
I4 Pb2 I11 . . 1_556 94.87(9) ?
I5 Pb2 I5 . . 4_545 178.51(7) ?
I5 Pb2 I7 . . . 92.69(10) ?
I5 Pb2 I9 . . . 86.28(9) ?
I5 Pb2 I11 . . 1_556 91.46(12) ?
I5 Pb2 I7 4_545 . . 88.33(10) ?
I5 Pb2 I9 4_545 . . 92.67(9) ?
I5 Pb2 I11 4_545 . 1_556 89.70(12) ?
I7 Pb2 I9 . . . 87.75(8) ?
I7 Pb2 I11 . . 1_556 86.17(9) ?
I9 Pb2 I11 . . 1_556 173.41(13) ?
Pb1 I1 Pb1 . . 4_655 179.78(15) ?
Pb1 I1 N2 . . 2_665 84.42(8) ?
Pb1 I1 N3 . . 1_665 89.48(10) ?
Pb1 I1 N2 4_655 . 2_665 95.58(9) ?
Pb1 I1 N3 4_655 . 1_665 90.74(10) ?
N2 I1 N3 2_665 . 1_665 97.24(12) ?
Pb1 I2 Pb1 3_455 . 4_545 158.709(12) ?
Pb1 I2 N3 3_455 . . 102.10(5) ?
Pb1 I2 N3 3_455 . 2_555 89.15(5) ?
Pb1 I2 N3 4_545 . . 89.15(5) ?
Pb1 I2 N3 4_545 . 2_555 102.10(5) ?
N3 I2 N3 . . 2_555 116.41(5) ?
Pb3 I3 Pb4 3_455 . 3_455 159.17(18) ?
Pb3 I3 N1 3_455 . 3_445 88.69(10) ?
Pb3 I3 N1 3_455 . 4_555 87.78(10) ?
Pb4 I3 N1 3_455 . 3_445 104.32(13) ?
Pb4 I3 N1 3_455 . 4_555 105.90(13) ?
N1 I3 N1 3_445 . 4_555 98.47(12) ?
Pb2 I4 Pb2 . . 2_555 149.155(15) ?
Pb2 I4 N5 . . 3_455 107.38(5) ?
Pb2 I4 N5 . . 4_545 87.99(5) ?
Pb2 I4 N5 2_555 . 3_455 87.99(5) ?
Pb2 I4 N5 2_555 . 4_545 107.38(5) ?
N5 I4 N5 3_455 . 4_545 120.57(5) ?
Pb2 I5 Pb2 . . 4_555 178.693(11) ?
Pb2 I5 N2 . . 1_556 93.62(8) ?
Pb2 I5 N5 . . 4_545 89.90(10) ?
Pb2 I5 N2 4_555 . 1_556 85.33(8) ?
Pb2 I5 N5 4_555 . 4_545 91.08(10) ?
N2 I5 N5 1_556 . 4_545 101.93(12) ?
Pb1 I6 Pb1 3_455 . 4_645 156.694(12) ?
Pb1 I6 N2 3_455 . 3_555 109.36(5) ?
Pb1 I6 N2 3_455 . 4_545 85.88(4) ?
Pb1 I6 N2 4_645 . 3_555 85.88(4) ?
Pb1 I6 N2 4_645 . 4_545 109.36(5) ?
N2 I6 N2 3_555 . 4_545 100.03(5) ?
Pb2 I7 Pb2 . . 2_655 151.355(14) ?
Pb2 I7 N2 . . 3_556 109.84(4) ?
Pb2 I7 N2 . . 4_546 89.12(4) ?
Pb2 I7 N2 2_655 . 3_556 89.12(4) ?
Pb2 I7 N2 2_655 . 4_546 109.84(4) ?
N2 I7 N2 3_556 . 4_546 98.19(5) ?
Pb3 I8 N4 . . 3_565 86.68(8) ?
Pb3 I8 N4 . . 4_645 95.10(8) ?
N4 I8 N4 3_565 . 4_645 104.19(10) ?
Pb2 I9 N5 . . 1_545 92.04(9) ?
Pb2 I9 N5 . . 2_665 101.55(8) ?
N5 I9 N5 1_545 . 2_665 109.29(10) ?
Pb1 I10 Pb4 3_455 . 3_455 160.28(7) ?
Pb1 I10 N3 3_455 . 3_545 87.15(6) ?
Pb4 I10 N3 3_455 . 3_545 104.03(6) ?
Pb1 I11 Pb2 3_455 . 1_554 158.75(18) ?
Pb1 I11 N2 3_455 . . 94.95(13) ?
Pb1 I11 N2 3_455 . 4_545 81.71(11) ?
Pb2 I11 N2 1_554 . . 94.03(12) ?
Pb2 I11 N2 1_554 . 4_545 83.40(11) ?
N2 I11 N2 . . 4_545 160.45(16) ?
I3 Pb3 I8 3_555 . . 172.94(13) ?
I3 Pb3 I13 3_555 . 3_555 85.70(9) ?
I3 Pb3 I14 3_555 . 3_555 94.74(9) ?
I3 Pb3 I18 3_555 . . 90.72(12) ?
I3 Pb3 I18 3_555 . 4_655 89.47(12) ?
I8 Pb3 I13 . . 3_555 88.22(8) ?
I8 Pb3 I14 . . 3_555 91.57(7) ?
I8 Pb3 I18 . . . 85.96(9) ?
I8 Pb3 I18 . . 4_655 93.97(9) ?
I13 Pb3 I14 3_555 . 3_555 176.13(8) ?
I13 Pb3 I18 3_555 . . 92.69(10) ?
I13 Pb3 I18 3_555 . 4_655 88.51(10) ?
I14 Pb3 I18 3_555 . . 91.15(10) ?
I14 Pb3 I18 3_555 . 4_655 87.65(10) ?
I18 Pb3 I18 . . 4_655 178.80(13) ?
C3 I12 N4 . . . 46.65(10) ?
C3 I12 N5 . . . 42.87(10) ?
N4 I12 N5 . . . 89.30(7) ?
I3 Pb4 I10 3_555 . 3_555 179.15(14) ?
I3 Pb4 I15 3_555 . . 90.57(9) ?
I3 Pb4 I16 3_555 . 3_555 91.63(10) ?
I3 Pb4 I17 3_555 . . 89.86(13) ?
I3 Pb4 I17 3_555 . 4_655 91.40(13) ?
I10 Pb4 I15 3_555 . . 89.80(5) ?
I10 Pb4 I16 3_555 . 3_555 88.02(4) ?
I10 Pb4 I17 3_555 . . 89.37(6) ?
I10 Pb4 I17 3_555 . 4_655 89.37(6) ?
I15 Pb4 I16 . . 3_555 177.57(4) ?
I15 Pb4 I17 . . . 90.66(12) ?
I15 Pb4 I17 . . 4_655 89.28(12) ?
I16 Pb4 I17 3_555 . . 90.38(12) ?
I16 Pb4 I17 3_555 . 4_655 89.63(12) ?
I17 Pb4 I17 . . 4_655 178.74(4) ?
Pb3 I13 Pb3 3_455 . 4_645 150.441(15) ?
Pb3 I13 N1 3_455 . . 99.12(5) ?
Pb3 I13 N1 3_455 . 2_655 95.04(5) ?
Pb3 I13 N1 4_645 . . 95.04(5) ?
Pb3 I13 N1 4_645 . 2_655 99.12(5) ?
N1 I13 N1 . . 2_655 122.26(4) ?
Pb3 I14 Pb3 3_455 . 4_545 149.480(15) ?
Pb3 I14 N4 3_455 . 3_455 101.10(5) ?
Pb3 I14 N4 3_455 . 4_545 90.89(5) ?
Pb3 I14 N4 4_545 . 3_455 90.89(5) ?
Pb3 I14 N4 4_545 . 4_545 101.10(5) ?
N4 I14 N4 3_455 . 4_545 133.46(5) ?
Pb4 I15 Pb4 . . 2_765 160.484(11) ?
Pb4 I16 Pb4 3_455 . 4_545 156.120(13) ?
Pb4 I17 Pb4 . . 4_645 178.73(6) ?
Pb3 I18 Pb3 . . 4_645 179.49(11) ?
Pb3 I18 N1 . . 2_655 86.57(9) ?
Pb3 I18 N1 . . 4_655 89.97(10) ?
Pb3 I18 N4 . . 2_665 92.64(10) ?
Pb3 I18 N4 . . 4_645 84.53(10) ?
Pb3 I18 N1 4_645 . 2_655 93.40(10) ?
Pb3 I18 N1 4_645 . 4_655 89.52(10) ?
Pb3 I18 N4 4_645 . 2_665 87.85(10) ?
Pb3 I18 N4 4_645 . 4_645 95.44(11) ?
N1 I18 N1 2_655 . 4_655 98.74(4) ?
N1 I18 N4 2_655 . 2_665 79.62(10) ?
N1 I18 N4 2_655 . 4_645 169.47(11) ?
N1 I18 N4 4_655 . 2_665 176.81(12) ?
N1 I18 N4 4_655 . 4_645 75.67(10) ?
N4 I18 N4 2_665 . 4_645 106.38(5) ?
I3 N1 I3 3_545 . 4_545 78.94(12) ?
I3 N1 I13 3_545 . . 138.34(9) ?
I3 N1 I18 3_545 . 2_655 128.35(9) ?
I3 N1 I18 3_545 . 4_645 68.47(8) ?
I3 N1 C1 3_545 . . 71.38(13) ?
I3 N1 H1n1 3_545 . . 67.50(16) ?
I3 N1 H2n1 3_545 . . 72.77(16) ?
I3 N1 H3n1 3_545 . . 176.8(2) ?
I3 N1 I13 4_545 . . 136.33(9) ?
I3 N1 I18 4_545 . 2_655 69.93(8) ?
I3 N1 I18 4_545 . 4_645 126.67(10) ?
I3 N1 C1 4_545 . . 72.51(13) ?
I3 N1 H1n1 4_545 . . 45.53(13) ?
I3 N1 H2n1 4_545 . . 148.8(2) ?
I3 N1 H3n1 4_545 . . 98.34(19) ?
I13 N1 I18 . . 2_655 67.91(6) ?
I13 N1 I18 . . 4_645 71.29(6) ?
I13 N1 C1 . . . 131.40(15) ?
I13 N1 H1n1 . . . 117.42(14) ?
I13 N1 H2n1 . . . 66.74(13) ?
I13 N1 H3n1 . . . 43.39(12) ?
I18 N1 I18 2_655 . 4_645 98.65(7) ?
I18 N1 C1 2_655 . . 131.11(16) ?
I18 N1 H1n1 2_655 . . 61.19(15) ?
I18 N1 H2n1 2_655 . . 118.92(14) ?
I18 N1 H3n1 2_655 . . 48.73(13) ?
I18 N1 C1 4_645 . . 129.02(16) ?
I18 N1 H1n1 4_645 . . 82.59(15) ?
I18 N1 H2n1 4_645 . . 28.29(11) ?
I18 N1 H3n1 4_645 . . 112.38(15) ?
C1 N1 H1n1 . . . 109.5(2) ?
C1 N1 H2n1 . . . 109.5(2) ?
C1 N1 H3n1 . . . 109.5(2) ?
H1n1 N1 H2n1 . . . 109.5(2) ?
H1n1 N1 H3n1 . . . 109.4(2) ?
H2n1 N1 H3n1 . . . 109.5(2) ?
I1 N2 I5 2_665 . 1_554 108.11(9) ?
I1 N2 I6 2_665 . 3_455 71.79(7) ?
I1 N2 I7 2_665 . 3_454 136.00(8) ?
I1 N2 I11 2_665 . . 69.84(8) ?
I1 N2 I11 2_665 . 4_555 69.40(8) ?
I1 N2 C2 2_665 . . 126.94(17) ?
I1 N2 H1n2 2_665 . . 108.33(17) ?
I1 N2 H2n2 2_665 . . 20.88(12) ?
I1 N2 H3n2 2_665 . . 91.09(16) ?
I5 N2 I6 1_554 . 3_455 134.41(8) ?
I5 N2 I7 1_554 . 3_454 68.40(7) ?
I5 N2 I11 1_554 . . 71.77(8) ?
I5 N2 I11 1_554 . 4_555 68.97(8) ?
I5 N2 C2 1_554 . . 121.85(17) ?
I5 N2 H1n2 1_554 . . 62.67(15) ?
I5 N2 H2n2 1_554 . . 127.92(15) ?
I5 N2 H3n2 1_554 . . 46.91(15) ?
I6 N2 I7 3_455 . 3_454 80.89(4) ?
I6 N2 I11 3_455 . . 139.31(7) ?
I6 N2 I11 3_455 . 4_555 68.86(7) ?
I6 N2 C2 3_455 . . 84.47(13) ?
I6 N2 H1n2 3_455 . . 73.98(15) ?
I6 N2 H2n2 3_455 . . 54.44(13) ?
I6 N2 H3n2 3_455 . . 162.53(18) ?
I7 N2 I11 3_454 . . 137.92(7) ?
I7 N2 I11 3_454 . 4_555 68.81(7) ?
I7 N2 C2 3_454 . . 82.32(13) ?
I7 N2 H1n2 3_454 . . 29.11(11) ?
I7 N2 H2n2 3_454 . . 130.82(18) ?
I7 N2 H3n2 3_454 . . 110.70(19) ?
I11 N2 I11 . . 4_555 108.69(12) ?
I11 N2 C2 . . . 108.30(16) ?
I11 N2 H1n2 . . . 131.36(17) ?
I11 N2 H2n2 . . . 85.10(15) ?
I11 N2 H3n2 . . . 27.23(13) ?
I11 N2 C2 4_555 . . 142.94(17) ?
I11 N2 H1n2 4_555 . . 39.74(13) ?
I11 N2 H2n2 4_555 . . 75.92(13) ?
I11 N2 H3n2 4_555 . . 102.37(16) ?
C2 N2 H1n2 . . . 109.5(2) ?
C2 N2 H2n2 . . . 109.5(2) ?
C2 N2 H3n2 . . . 109.5(2) ?
H1n2 N2 H2n2 . . . 109.5(2) ?
H1n2 N2 H3n2 . . . 109.5(3) ?
H2n2 N2 H3n2 . . . 109.5(2) ?
I1 N3 I2 1_445 . . 72.44(7) ?
I1 N3 I10 1_445 . 3_445 73.16(7) ?
I1 N3 C6 1_445 . . 171.66(17) ?
I1 N3 H1n3 1_445 . . 75.92(15) ?
I1 N3 H2n3 1_445 . . 73.65(15) ?
I1 N3 H3n3 1_445 . . 62.31(14) ?
I2 N3 I10 . . 3_445 145.47(6) ?
I2 N3 C6 . . . 99.36(13) ?
I2 N3 H1n3 . . . 113.42(18) ?
I2 N3 H2n3 . . . 115.09(16) ?
I2 N3 H3n3 . . . 10.15(11) ?
I10 N3 C6 3_445 . . 114.93(15) ?
I10 N3 H1n3 3_445 . . 59.95(13) ?
I10 N3 H2n3 3_445 . . 50.82(13) ?
I10 N3 H3n3 3_445 . . 135.32(16) ?
C6 N3 H1n3 . . . 109.5(2) ?
C6 N3 H2n3 . . . 109.5(2) ?
C6 N3 H3n3 . . . 109.5(2) ?
H1n3 N3 H2n3 . . . 109.5(2) ?
H1n3 N3 H3n3 . . . 109.5(3) ?
H2n3 N3 H3n3 . . . 109.5(2) ?
N1 C1 H1c1 . . . 109.5(2) ?
N1 C1 H2c1 . . . 109.4(2) ?
N1 C1 H3c1 . . . 109.48(19) ?
H1c1 C1 H2c1 . . . 109.4(2) ?
H1c1 C1 H3c1 . . . 109.5(2) ?
H2c1 C1 H3c1 . . . 109.5(2) ?
N2 C2 H1c2 . . . 109.5(2) ?
N2 C2 H2c2 . . . 109.5(2) ?
N2 C2 H3c2 . . . 109.5(2) ?
H1c2 C2 H2c2 . . . 109.5(2) ?
H1c2 C2 H3c2 . . . 109.5(2) ?
H2c2 C2 H3c2 . . . 109.5(2) ?
I12 C3 C4 . . . 109.5(3) ?
I12 C3 C5 . . . 106.4(3) ?
I12 C3 H1c3 . . . 107.5(3) ?
C4 C3 C5 . . . 94.1(3) ?
C4 C3 H1c3 . . . 117.8(4) ?
C5 C3 H1c3 . . . 120.4(3) ?
C3 C4 N4 . . . 110.7(3) ?
C3 C4 H1c4 . . . 109.5(3) ?
C3 C4 H2c4 . . . 109.5(2) ?
N4 C4 H1c4 . . . 109.5(2) ?
N4 C4 H2c4 . . . 109.4(2) ?
H1c4 C4 H2c4 . . . 108.3(4) ?
I8 N4 I8 3_465 . 4_655 72.89(9) ?
I8 N4 I12 3_465 . . 121.61(6) ?
I8 N4 I14 3_465 . 3_555 150.01(8) ?
I8 N4 I18 3_465 . 2_665 74.12(8) ?
I8 N4 I18 3_465 . 4_655 125.32(9) ?
I8 N4 C4 3_465 . . 77.57(15) ?
I8 N4 H1n4 3_465 . . 82.53(17) ?
I8 N4 H2n4 3_465 . . 52.77(15) ?
I8 N4 H3n4 3_465 . . 161.9(2) ?
I8 N4 I12 4_655 . . 82.68(7) ?
I8 N4 I14 4_655 . 3_555 133.41(9) ?
I8 N4 I18 4_655 . 2_665 130.35(10) ?
I8 N4 I18 4_655 . 4_655 66.82(8) ?
I8 N4 C4 4_655 . . 112.01(15) ?
I8 N4 H1n4 4_655 . . 124.90(19) ?
I8 N4 H2n4 4_655 . . 21.51(13) ?
I8 N4 H3n4 4_655 . . 89.06(17) ?
I12 N4 I14 . . 3_555 81.32(6) ?
I12 N4 I18 . . 2_665 146.84(10) ?
I12 N4 I18 . . 4_655 88.50(7) ?
I12 N4 C4 . . . 63.82(15) ?
I12 N4 H1n4 . . . 149.6(2) ?
I12 N4 H2n4 . . . 100.41(16) ?
I12 N4 H3n4 . . . 52.99(12) ?
I14 N4 I18 3_555 . 2_665 76.55(7) ?
I14 N4 I18 3_555 . 4_655 69.29(7) ?
I14 N4 C4 3_555 . . 99.33(15) ?
I14 N4 H1n4 3_555 . . 70.28(16) ?
I14 N4 H2n4 3_555 . . 148.74(18) ?
I14 N4 H3n4 3_555 . . 47.16(14) ?
I18 N4 I18 2_665 . 4_655 106.03(8) ?
I18 N4 C4 2_665 . . 95.65(17) ?
I18 N4 H1n4 2_665 . . 14.65(13) ?
I18 N4 H2n4 2_665 . . 111.34(18) ?
I18 N4 H3n4 2_665 . . 120.33(17) ?
I18 N4 C4 4_655 . . 151.76(18) ?
I18 N4 H1n4 4_655 . . 91.37(15) ?
I18 N4 H2n4 4_655 . . 79.52(16) ?
I18 N4 H3n4 4_655 . . 43.66(13) ?
C4 N4 H1n4 . . . 109.5(2) ?
C4 N4 H2n4 . . . 109.5(2) ?
C4 N4 H3n4 . . . 109.5(2) ?
H1n4 N4 H2n4 . . . 109.5(3) ?
H1n4 N4 H3n4 . . . 109.5(2) ?
H2n4 N4 H3n4 . . . 109.5(3) ?
C3 C5 N5 . . . 94.0(3) ?
C3 C5 H1c5 . . . 109.5(2) ?
C3 C5 H2c5 . . . 109.5(3) ?
N5 C5 H1c5 . . . 109.5(2) ?
N5 C5 H2c5 . . . 109.5(2) ?
H1c5 C5 H2c5 . . . 121.4(4) ?
I4 N5 I5 3_555 . 4_555 75.49(7) ?
I4 N5 I9 3_555 . 1_565 148.34(7) ?
I4 N5 I9 3_555 . 2_665 122.42(8) ?
I4 N5 I12 3_555 . . 82.93(6) ?
I4 N5 C5 3_555 . . 102.10(14) ?
I4 N5 H1n5 3_555 . . 106.44(17) ?
I4 N5 H2n5 3_555 . . 119.44(16) ?
I4 N5 H3n5 3_555 . . 10.31(11) ?
I5 N5 I9 4_555 . 1_565 73.36(8) ?
I5 N5 I9 4_555 . 2_665 119.99(9) ?
I5 N5 I12 4_555 . . 155.77(10) ?
I5 N5 C5 4_555 . . 106.02(18) ?
I5 N5 H1n5 4_555 . . 143.01(18) ?
I5 N5 H2n5 4_555 . . 46.97(14) ?
I5 N5 H3n5 4_555 . . 66.94(15) ?
I9 N5 I9 1_565 . 2_665 70.49(9) ?
I9 N5 I12 1_565 . . 128.73(7) ?
I9 N5 C5 1_565 . . 91.83(15) ?
I9 N5 H1n5 1_565 . . 95.16(17) ?
I9 N5 H2n5 1_565 . . 29.26(12) ?
I9 N5 H3n5 1_565 . . 138.65(17) ?
I9 N5 I12 2_665 . . 80.94(7) ?
I9 N5 C5 2_665 . . 121.19(15) ?
I9 N5 H1n5 2_665 . . 27.72(14) ?
I9 N5 H2n5 2_665 . . 81.74(17) ?
I9 N5 H3n5 2_665 . . 120.68(18) ?
I12 N5 C5 . . . 67.64(16) ?
I12 N5 H1n5 . . . 54.30(13) ?
I12 N5 H2n5 . . . 156.91(19) ?
I12 N5 H3n5 . . . 92.50(16) ?
C5 N5 H1n5 . . . 109.5(2) ?
C5 N5 H2n5 . . . 109.5(2) ?
C5 N5 H3n5 . . . 109.5(2) ?
H1n5 N5 H2n5 . . . 109.5(3) ?
H1n5 N5 H3n5 . . . 109.4(3) ?
H2n5 N5 H3n5 . . . 109.5(2) ?
N3 C6 H1c6 . . . 109.5(2) ?
N3 C6 H2c6 . . . 109.5(2) ?
N3 C6 H3c6 . . . 109.47(19) ?
H1c6 C6 H2c6 . . . 109.5(2) ?
H1c6 C6 H3c6 . . . 109.5(3) ?
H2c6 C6 H3c6 . . . 109.5(2) ?

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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
? ? ? ? ? ? ? ? ? ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
? ? ? ? ? ? ? ? ? ? ?


#=======================================================================

# 11. STRUCTURE-FACTOR LIST



