# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry A.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_(CH3NH2)4PBI2
_audit_block_doi                 10.5517/ccdc.csd.cc230jm9
_database_code_depnum_ccdc_archive 'CCDC 1936930'
loop_
_audit_author_name
_audit_author_address
'Harald Hillebrecht'
;Freiburg University Institute for Inorganic Chemsitry
Germany
;
_audit_update_record             
;
2020-04-20 deposited with the CCDC.	2020-05-06 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2014/7
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C4 H20 I2 N4 Pb'
_chemical_formula_weight         585.23

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'

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

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

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

_cell_length_a                   8.5684(2)
_cell_length_b                   12.6121(3)
_cell_length_c                   13.3607(3)
_cell_angle_alpha                90
_cell_angle_beta                 98.8770(10)
_cell_angle_gamma                90
_cell_volume                     1426.54(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    89003
_cell_measurement_theta_min      4
_cell_measurement_theta_max      43.7

_exptl_crystal_description       rod
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.725
_exptl_crystal_F_000             1040
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_exptl_absorpt_coefficient_mu    16.122
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  .453
_exptl_absorpt_correction_T_max  .630
_exptl_absorpt_process_details   Program_SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         microsource
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            89003
_diffrn_reflns_av_unetI/netI     0.0390
_diffrn_reflns_av_R_equivalents  0.0622
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.233
_diffrn_reflns_theta_max         43.705
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             10940
_reflns_number_gt                8601
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Diamond (Crystal impact, 2005)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0127P)²+2.2762P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10940
_refine_ls_number_parameters     104
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0292
_refine_ls_wR_factor_ref         0.0498
_refine_ls_wR_factor_gt          0.0463
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb Pb 0.66363(2) 0.33393(2) 0.26437(2) 0.01222(2) Uani 1 1 d . . . . .
I2 I 1.17761(2) 0.57955(2) 0.34860(2) 0.01666(3) Uani 1 1 d . . . . .
I1 I 0.49178(2) 0.19258(2) 0.42346(2) 0.01921(3) Uani 1 1 d . . . . .
N1 N 0.5956(2) 0.45972(14) 0.38937(15) 0.0142(3) Uani 1 1 d . . . . .
H11 H 0.4789 0.4630 0.3817 0.017 Uiso 1 1 calc R U . . .
H12 H 0.6333 0.4298 0.4573 0.017 Uiso 1 1 calc R U . . .
N2 N 0.7944(2) 0.49024(16) 0.19191(15) 0.0159(3) Uani 1 1 d . . . . .
H21 H 0.7177 0.5490 0.1768 0.019 Uiso 1 1 calc R U . . .
H22 H 0.8842 0.5159 0.2416 0.019 Uiso 1 1 calc R U . . .
N3 N 0.9193(3) 0.34432(16) 0.39536(17) 0.0186(4) Uani 1 1 d . . . . .
H31 H 0.9883 0.4009 0.3752 0.022 Uiso 1 1 calc R U . . .
H32 H 0.8920 0.3630 0.4625 0.022 Uiso 1 1 calc R U . . .
N4 N 0.4074(3) 0.42591(17) 0.17066(16) 0.0190(4) Uani 1 1 d . . . . .
H41 H 0.3830 0.4894 0.2090 0.023 Uiso 1 1 calc R U . . .
H42 H 0.4243 0.4489 0.1023 0.023 Uiso 1 1 calc R U . . .
C1 C 0.6547(3) 0.56977(18) 0.38849(19) 0.0198(4) Uani 1 1 d . . . . .
H111 H 0.7705 0.5693 0.3999 0.030 Uiso 1 1 calc R U . . .
H112 H 0.6165 0.6105 0.4423 0.030 Uiso 1 1 calc R U . . .
H113 H 0.6163 0.6024 0.3227 0.030 Uiso 1 1 calc R U . . .
C2 C 0.8507(4) 0.4558(2) 0.0986(2) 0.0268(5) Uani 1 1 d . . . . .
H211 H 0.9063 0.3880 0.1106 0.040 Uiso 1 1 calc R U . . .
H212 H 0.9230 0.5092 0.0785 0.040 Uiso 1 1 calc R U . . .
H213 H 0.7605 0.4473 0.0445 0.040 Uiso 1 1 calc R U . . .
C3 C 1.0052(4) 0.2429(2) 0.4028(3) 0.0311(6) Uani 1 1 d . . . . .
H311 H 0.9353 0.1862 0.4194 0.047 Uiso 1 1 calc R U . . .
H312 H 1.0974 0.2478 0.4560 0.047 Uiso 1 1 calc R U . . .
H313 H 1.0400 0.2272 0.3379 0.047 Uiso 1 1 calc R U . . .
C4 C 0.2756(3) 0.3511(2) 0.1623(2) 0.0253(5) Uani 1 1 d . . . . .
H411 H 0.3057 0.2847 0.1322 0.038 Uiso 1 1 calc R U . . .
H412 H 0.1836 0.3816 0.1193 0.038 Uiso 1 1 calc R U . . .
H413 H 0.2492 0.3368 0.2298 0.038 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
Pb N1 2.4386(18) . ?
Pb N2 2.5325(19) . ?
Pb N3 2.588(2) . ?
Pb N4 2.624(2) . ?
Pb I1 3.29096(18) . ?
N1 C1 1.478(3) . ?
N1 H11 0.9900 . ?
N1 H12 0.9900 . ?
N2 C2 1.470(3) . ?
N2 H21 0.9900 . ?
N2 H22 0.9900 . ?
N3 C3 1.471(3) . ?
N3 H31 0.9900 . ?
N3 H32 0.9900 . ?
N4 C4 1.463(3) . ?
N4 H41 0.9900 . ?
N4 H42 0.9900 . ?
C1 H111 0.9800 . ?
C1 H112 0.9800 . ?
C1 H113 0.9800 . ?
C2 H211 0.9800 . ?
C2 H212 0.9800 . ?
C2 H213 0.9800 . ?
C3 H311 0.9800 . ?
C3 H312 0.9800 . ?
C3 H313 0.9800 . ?
C4 H411 0.9800 . ?
C4 H412 0.9800 . ?
C4 H413 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
N1 Pb N2 85.53(6) . . ?
N1 Pb N3 76.75(7) . . ?
N2 Pb N3 80.84(7) . . ?
N1 Pb N4 76.60(7) . . ?
N2 Pb N4 81.97(7) . . ?
N3 Pb N4 149.20(7) . . ?
N1 Pb I1 74.45(4) . . ?
N2 Pb I1 159.55(5) . . ?
N3 Pb I1 90.40(5) . . ?
N4 Pb I1 97.06(5) . . ?
C1 N1 Pb 119.14(14) . . ?
C1 N1 H11 107.5 . . ?
Pb N1 H11 107.5 . . ?
C1 N1 H12 107.5 . . ?
Pb N1 H12 107.5 . . ?
H11 N1 H12 107.0 . . ?
C2 N2 Pb 108.48(16) . . ?
C2 N2 H21 110.0 . . ?
Pb N2 H21 110.0 . . ?
C2 N2 H22 110.0 . . ?
Pb N2 H22 110.0 . . ?
H21 N2 H22 108.4 . . ?
C3 N3 Pb 111.34(17) . . ?
C3 N3 H31 109.4 . . ?
Pb N3 H31 109.4 . . ?
C3 N3 H32 109.4 . . ?
Pb N3 H32 109.4 . . ?
H31 N3 H32 108.0 . . ?
C4 N4 Pb 109.30(16) . . ?
C4 N4 H41 109.8 . . ?
Pb N4 H41 109.8 . . ?
C4 N4 H42 109.8 . . ?
Pb N4 H42 109.8 . . ?
H41 N4 H42 108.3 . . ?
N1 C1 H111 109.5 . . ?
N1 C1 H112 109.5 . . ?
H111 C1 H112 109.5 . . ?
N1 C1 H113 109.5 . . ?
H111 C1 H113 109.5 . . ?
H112 C1 H113 109.5 . . ?
N2 C2 H211 109.5 . . ?
N2 C2 H212 109.5 . . ?
H211 C2 H212 109.5 . . ?
N2 C2 H213 109.5 . . ?
H211 C2 H213 109.5 . . ?
H212 C2 H213 109.5 . . ?
N3 C3 H311 109.5 . . ?
N3 C3 H312 109.5 . . ?
H311 C3 H312 109.5 . . ?
N3 C3 H313 109.5 . . ?
H311 C3 H313 109.5 . . ?
H312 C3 H313 109.5 . . ?
N4 C4 H411 109.5 . . ?
N4 C4 H412 109.5 . . ?
H411 C4 H412 109.5 . . ?
N4 C4 H413 109.5 . . ?
H411 C4 H413 109.5 . . ?
H412 C4 H413 109.5 . . ?

_refine_diff_density_max         1.865
_refine_diff_density_min         -2.648
_refine_diff_density_rms         0.255

_shelxl_version_number           2013-4



####################################################################### 
# 
# 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_HH_MD_88_3_0m
_database_code_depnum_ccdc_archive 'CCDC 1997919'
loop_
_audit_author_name
_audit_author_address
'Harald Hillebrecht'
;Freiburg University Institute for Inorganic Chemsitry
Germany
;
_audit_update_record             
;
2020-04-20 deposited with the CCDC.	2020-05-06 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C7 H42 I9 N7 Pb2'
_chemical_formula_weight         1780.95

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   13.7676(14)
_cell_length_b                   14.8730(14)
_cell_length_c                   19.0855(19)
_cell_angle_alpha                90
_cell_angle_beta                 110.585(4)
_cell_angle_gamma                90
_cell_volume                     3658.5(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       platelet
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.233
_exptl_crystal_F_000             3096
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    16.795
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3735
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6492
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         4.408
_diffrn_reflns_theta_max         29.991
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.420
_diffrn_measured_fraction_theta_full 0.462
_diffrn_reflns_Laue_measured_fraction_max 0.420
_diffrn_reflns_Laue_measured_fraction_full 0.462
_diffrn_reflns_point_group_measured_fraction_max 0.420
_diffrn_reflns_point_group_measured_fraction_full 0.462
_reflns_number_total             4470
_reflns_number_gt                3751
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Diamond (Crystal impact, 2005)'
_computing_publication_material  'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0788P)²+94.7584P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.00024(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4470
_refine_ls_number_parameters     171
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0516
_refine_ls_wR_factor_ref         0.1382
_refine_ls_wR_factor_gt          0.1320
_refine_ls_goodness_of_fit_ref   0.939
_refine_ls_restrained_S_all      0.939
_refine_ls_shift/su_max          0.124
_refine_ls_shift/su_mean         0.003

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 0.17911(4) 0.73807(4) 0.38239(4) 0.0191(2) Uani 1 1 d . . . . .
Pb2 Pb 0.47921(4) 0.74635(5) 0.37251(5) 0.0209(2) Uani 1 1 d . . . . .
I1 I 0.40245(7) 0.67405(8) 0.50728(8) 0.0241(4) Uani 1 1 d . . . . .
I2 I 0.26538(9) 0.63840(9) 0.26000(9) 0.0285(4) Uani 1 1 d . . . . .
I3 I 0.31489(7) 0.90996(9) 0.35533(9) 0.0292(4) Uani 1 1 d . . . . .
I6 I 0.07296(10) 0.56227(10) 0.40970(10) 0.0364(5) Uani 1 1 d . . . . .
I4 I 0.14837(8) 0.83938(9) 0.51676(9) 0.0315(4) Uani 1 1 d . . . . .
I5 I -0.01649(8) 0.81555(10) 0.25701(9) 0.0369(4) Uani 1 1 d . . . . .
I8 I 0.63882(7) 0.85441(9) 0.50211(10) 0.0382(5) Uani 1 1 d . . . . .
I9 I 0.61862(8) 0.57183(9) 0.39662(11) 0.0450(5) Uani 1 1 d . . . . .
I7 I 0.54311(10) 0.83760(11) 0.24850(10) 0.0400(5) Uani 1 1 d . . . . .
C1 C -0.2916(13) 0.8944(14) 0.1243(15) 0.028(3) Uiso 1 1 d . . . . .
H1A H -0.227525 0.917035 0.119237 0.043 Uiso 1 1 calc R U . . .
H1B H -0.315799 0.841599 0.092214 0.043 Uiso 1 1 calc R U . . .
H1C H -0.278099 0.877641 0.176568 0.043 Uiso 1 1 calc R U . . .
N1 N 0.6289(12) 0.5355(13) 0.6019(13) 0.035(3) Uiso 1 1 d . . . . .
H1D H 0.643766 0.492535 0.638146 0.053 Uiso 1 1 calc R U . . .
H1E H 0.627670 0.510217 0.558206 0.053 Uiso 1 1 calc R U . . .
H1F H 0.565859 0.560098 0.595529 0.053 Uiso 1 1 calc R U . . .
N2 N 0.2654(11) 0.8521(12) 0.1396(12) 0.030(3) Uiso 1 1 d . . . . .
H2A H 0.299139 0.887824 0.116883 0.044 Uiso 1 1 calc R U . . .
H2B H 0.250687 0.798241 0.115471 0.044 Uiso 1 1 calc R U . . .
H2C H 0.306484 0.843000 0.188155 0.044 Uiso 1 1 calc R U . . .
C2 C 0.1714(14) 0.8945(16) 0.1369(16) 0.035(4) Uiso 1 1 d . . . . .
H2D H 0.127333 0.850753 0.150046 0.052 Uiso 1 1 calc R U . . .
H2E H 0.134909 0.917338 0.086299 0.052 Uiso 1 1 calc R U . . .
H2F H 0.187289 0.944505 0.172601 0.052 Uiso 1 1 calc R U . . .
N3 N 0.5815(12) 1.0813(13) 0.4385(12) 0.036(3) Uiso 1 1 d . . . . .
H3A H 0.646102 1.105493 0.458563 0.054 Uiso 1 1 calc R U . . .
H3B H 0.583614 1.022295 0.451557 0.054 Uiso 1 1 calc R U . . .
H3C H 0.537145 1.111338 0.455982 0.054 Uiso 1 1 calc R U . . .
C3 C 0.5463(17) 1.0887(18) 0.3586(17) 0.044(5) Uiso 1 1 d . . . . .
H3D H 0.479350 1.120001 0.340684 0.067 Uiso 1 1 calc R U . . .
H3E H 0.538243 1.028528 0.336441 0.067 Uiso 1 1 calc R U . . .
H3F H 0.597110 1.122801 0.344055 0.067 Uiso 1 1 calc R U . . .
C4 C -0.0963(13) 0.7934(15) 0.0422(14) 0.032(4) Uiso 1 1 d . . . . .
H4A H -0.031568 0.758896 0.057852 0.048 Uiso 1 1 calc R U . . .
H4B H -0.150754 0.757831 0.051122 0.048 Uiso 1 1 calc R U . . .
H4C H -0.085728 0.849396 0.070939 0.048 Uiso 1 1 calc R U . . .
N4 N 0.8731(13) 0.6861(14) 0.4644(13) 0.040(4) Uiso 1 1 d . . . . .
H4D H 0.857186 0.737945 0.437384 0.060 Uiso 1 1 calc R U . . .
H4E H 0.816587 0.649539 0.450845 0.060 Uiso 1 1 calc R U . . .
H4F H 0.926191 0.657904 0.455373 0.060 Uiso 1 1 calc R U . . .
N5 N -0.1789(17) 0.8308(17) 0.3747(15) 0.055(5) Uiso 1 1 d . . . . .
H5A H -0.155293 0.828820 0.335752 0.082 Uiso 1 1 calc R U . . .
H5B H -0.248889 0.822409 0.357207 0.082 Uiso 1 1 calc R U . . .
H5C H -0.147926 0.786594 0.408011 0.082 Uiso 1 1 calc R U . . .
C5 C -0.154(2) 0.918(2) 0.412(2) 0.054(6) Uiso 1 1 d . . . . .
H5D H -0.190762 0.924527 0.447152 0.081 Uiso 1 1 calc R U . . .
H5E H -0.176708 0.965950 0.373912 0.081 Uiso 1 1 calc R U . . .
H5F H -0.079456 0.922551 0.438251 0.081 Uiso 1 1 calc R U . . .
C6 C -0.2465(16) 0.6374(18) 0.2613(16) 0.042(5) Uiso 1 1 d . . . . .
H6A H -0.209098 0.586579 0.291504 0.063 Uiso 1 1 calc R U . . .
H6B H -0.321375 0.626222 0.244927 0.063 Uiso 1 1 calc R U . . .
H6C H -0.229825 0.692456 0.291482 0.063 Uiso 1 1 calc R U . . .
N6 N -0.219(4) 0.647(3) 0.202(3) 0.135(14) Uiso 1 1 d . . . . .
H6D H -0.197538 0.704550 0.199740 0.202 Uiso 1 1 calc R U . . .
H6E H -0.273499 0.634233 0.159776 0.202 Uiso 1 1 calc R U . . .
H6F H -0.165475 0.608618 0.205679 0.202 Uiso 1 1 calc R U . . .
C7 C -0.047(4) 0.936(3) 0.637(3) 0.106(13) Uiso 1 1 d . . . . .
H7D H -0.036137 0.993643 0.615395 0.160 Uiso 1 1 calc R U . . .
H7E H -0.109456 0.907110 0.602465 0.160 Uiso 1 1 calc R U . . .
H7F H 0.013261 0.897012 0.643658 0.160 Uiso 1 1 calc R U . . .
N7 N -0.059(3) 0.548(3) 0.211(3) 0.133(14) Uiso 1 1 d . . . . .
H7A H -0.049119 0.600417 0.236799 0.200 Uiso 1 1 calc R U . . .
H7B H -0.011097 0.506815 0.237356 0.200 Uiso 1 1 calc R U . . .
H7C H -0.123798 0.526654 0.203199 0.200 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 I5 3.1265(15) . ?
Pb1 I6 3.1271(14) . ?
Pb1 I4 3.1287(15) . ?
Pb1 I1 3.2999(13) . ?
Pb1 I3 3.3131(13) . ?
Pb1 I2 3.3189(14) . ?
Pb2 I7 3.1115(15) . ?
Pb2 I8 3.1158(17) . ?
Pb2 I9 3.1641(14) . ?
Pb2 I3 3.2597(12) . ?
Pb2 I1 3.2864(13) . ?
Pb2 I2 3.3779(16) . ?
C1 N1 1.46(3) 4_475 ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
N1 H1D 0.9100 . ?
N1 H1E 0.9100 . ?
N1 H1F 0.9100 . ?
N2 C2 1.42(2) . ?
N2 H2A 0.9100 . ?
N2 H2B 0.9100 . ?
N2 H2C 0.9100 . ?
C2 H2D 0.9800 . ?
C2 H2E 0.9800 . ?
C2 H2F 0.9800 . ?
N3 C3 1.43(4) . ?
N3 H3A 0.9100 . ?
N3 H3B 0.9100 . ?
N3 H3C 0.9100 . ?
C3 H3D 0.9800 . ?
C3 H3E 0.9800 . ?
C3 H3F 0.9800 . ?
C4 N4 1.43(3) 4_475 ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
N4 H4D 0.9100 . ?
N4 H4E 0.9100 . ?
N4 H4F 0.9100 . ?
N5 C5 1.46(4) . ?
N5 H5A 0.9100 . ?
N5 H5B 0.9100 . ?
N5 H5C 0.9100 . ?
C5 H5D 0.9800 . ?
C5 H5E 0.9800 . ?
C5 H5F 0.9800 . ?
C6 N6 1.33(4) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
N6 H6D 0.9100 . ?
N6 H6E 0.9100 . ?
N6 H6F 0.9100 . ?
C7 N7 1.50(6) 4_576 ?
C7 H7D 0.9800 . ?
C7 H7E 0.9800 . ?
C7 H7F 0.9800 . ?
N7 H7A 0.9100 . ?
N7 H7B 0.9100 . ?
N7 H7C 0.9100 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I5 Pb1 I6 96.23(4) . . ?
I5 Pb1 I4 96.98(4) . . ?
I6 Pb1 I4 93.46(4) . . ?
I5 Pb1 I1 172.89(4) . . ?
I6 Pb1 I1 90.56(4) . . ?
I4 Pb1 I1 84.67(4) . . ?
I5 Pb1 I3 88.72(4) . . ?
I6 Pb1 I3 173.48(3) . . ?
I4 Pb1 I3 90.14(4) . . ?
I1 Pb1 I3 84.36(3) . . ?
I5 Pb1 I2 92.92(4) . . ?
I6 Pb1 I2 92.73(4) . . ?
I4 Pb1 I2 167.68(4) . . ?
I1 Pb1 I2 84.62(4) . . ?
I3 Pb1 I2 82.75(4) . . ?
I7 Pb2 I8 94.00(5) . . ?
I7 Pb2 I9 98.58(4) . . ?
I8 Pb2 I9 94.89(4) . . ?
I7 Pb2 I3 88.26(4) . . ?
I8 Pb2 I3 88.03(4) . . ?
I9 Pb2 I3 172.34(3) . . ?
I7 Pb2 I1 173.10(4) . . ?
I8 Pb2 I1 83.02(4) . . ?
I9 Pb2 I1 87.90(4) . . ?
I3 Pb2 I1 85.42(3) . . ?
I7 Pb2 I2 98.05(5) . . ?
I8 Pb2 I2 164.49(4) . . ?
I9 Pb2 I2 92.93(4) . . ?
I3 Pb2 I2 82.64(4) . . ?
I1 Pb2 I2 83.90(3) . . ?
Pb2 I1 Pb1 79.32(3) . . ?
Pb1 I2 Pb2 77.76(4) . . ?
Pb2 I3 Pb1 79.51(3) . . ?
N1 C1 H1A 109.5 4_475 . ?
N1 C1 H1B 109.5 4_475 . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 4_475 . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C1 N1 H1D 109.5 4_676 . ?
C1 N1 H1E 109.5 4_676 . ?
H1D N1 H1E 109.5 . . ?
C1 N1 H1F 109.5 4_676 . ?
H1D N1 H1F 109.5 . . ?
H1E N1 H1F 109.5 . . ?
C2 N2 H2A 109.5 . . ?
C2 N2 H2B 109.5 . . ?
H2A N2 H2B 109.5 . . ?
C2 N2 H2C 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
N2 C2 H2D 109.5 . . ?
N2 C2 H2E 109.5 . . ?
H2D C2 H2E 109.5 . . ?
N2 C2 H2F 109.5 . . ?
H2D C2 H2F 109.5 . . ?
H2E C2 H2F 109.5 . . ?
C3 N3 H3A 109.5 . . ?
C3 N3 H3B 109.5 . . ?
H3A N3 H3B 109.5 . . ?
C3 N3 H3C 109.5 . . ?
H3A N3 H3C 109.5 . . ?
H3B N3 H3C 109.5 . . ?
N3 C3 H3D 109.5 . . ?
N3 C3 H3E 109.5 . . ?
H3D C3 H3E 109.5 . . ?
N3 C3 H3F 109.5 . . ?
H3D C3 H3F 109.5 . . ?
H3E C3 H3F 109.5 . . ?
N4 C4 H4A 109.5 4_475 . ?
N4 C4 H4B 109.5 4_475 . ?
H4A C4 H4B 109.5 . . ?
N4 C4 H4C 109.5 4_475 . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C4 N4 H4D 109.5 4_676 . ?
C4 N4 H4E 109.5 4_676 . ?
H4D N4 H4E 109.5 . . ?
C4 N4 H4F 109.5 4_676 . ?
H4D N4 H4F 109.5 . . ?
H4E N4 H4F 109.5 . . ?
C5 N5 H5A 109.5 . . ?
C5 N5 H5B 109.5 . . ?
H5A N5 H5B 109.5 . . ?
C5 N5 H5C 109.5 . . ?
H5A N5 H5C 109.5 . . ?
H5B N5 H5C 109.5 . . ?
N5 C5 H5D 109.5 . . ?
N5 C5 H5E 109.5 . . ?
H5D C5 H5E 109.5 . . ?
N5 C5 H5F 109.5 . . ?
H5D C5 H5F 109.5 . . ?
H5E C5 H5F 109.5 . . ?
N6 C6 H6A 109.5 . . ?
N6 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N6 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C6 N6 H6D 109.5 . . ?
C6 N6 H6E 109.5 . . ?
H6D N6 H6E 109.5 . . ?
C6 N6 H6F 109.5 . . ?
H6D N6 H6F 109.5 . . ?
H6E N6 H6F 109.5 . . ?
N7 C7 H7D 109.5 4_576 . ?
N7 C7 H7E 109.5 4_576 . ?
H7D C7 H7E 109.5 . . ?
N7 C7 H7F 109.5 4_576 . ?
H7D C7 H7F 109.5 . . ?
H7E C7 H7F 109.5 . . ?
C7 N7 H7A 109.5 4_575 . ?
C7 N7 H7B 109.5 4_575 . ?
H7A N7 H7B 109.5 . . ?
C7 N7 H7C 109.5 4_575 . ?
H7A N7 H7C 109.5 . . ?
H7B N7 H7C 109.5 . . ?

_refine_diff_density_max         3.769
_refine_diff_density_min         -2.717
_refine_diff_density_rms         0.295



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Methylamine'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Hygroscopic
####################################################################### 
# 
# 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_(CH3NH2)62PbI2
_audit_block_doi                 10.5517/ccdc.csd.cc25235k
_database_code_depnum_ccdc_archive 'CCDC 1998017'
loop_
_audit_author_name
_audit_author_address
'Harald Hillebrecht'
;Freiburg University Institute for Inorganic Chemsitry
Germany
;
_audit_update_record             
;
2020-04-20 deposited with the CCDC.	2020-05-06 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C6 H30 I2 N6 Pb'
_chemical_formula_weight         647.35

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           225
_space_group_name_H-M_alt        'F m -3 m'
_space_group_name_Hall           '-F 4 2 3'

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

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

_cell_length_a                   12.487(7)
_cell_length_b                   12.487(7)
_cell_length_c                   12.487(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1947(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7344
_cell_measurement_theta_min      2
_cell_measurement_theta_max      30

_exptl_crystal_description       polyhedron
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.208
_exptl_crystal_F_000             1184
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    11.826
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.135
_exptl_absorpt_correction_T_max  0.424
_exptl_absorpt_process_details   Program_SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         microsource
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7297
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_av_R_equivalents  0.0845
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.825
_diffrn_reflns_theta_max         30.338
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measured_fraction_theta_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_point_group_measured_fraction_full 0.975
_reflns_number_total             187
_reflns_number_gt                179
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Diamond (Crystal impact, 2005)'
_computing_publication_material  'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0800P)²+200.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.0014(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         187
_refine_ls_number_parameters     8
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0651
_refine_ls_wR_factor_ref         0.1753
_refine_ls_wR_factor_gt          0.1740
_refine_ls_goodness_of_fit_ref   1.287
_refine_ls_restrained_S_all      1.287
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I I 0.2243(13) 0.2243(13) 0.2243(13) 0.0209(15) Uiso 0.080(5) 6 d S U P . .
IA I 0.250000 0.250000 0.250000 0.0209(15) Uiso 0.68(2) 24 d S U P . .
Pb Pb 0.000000 0.000000 0.000000 0.0177(8) Uiso 1 48 d S . P . .
C C 0.000000 0.000000 0.268(2) 0.089(9) Uiso 1 8 d S U P . .
N N 0.000000 0.000000 0.268(2) 0.089(9) Uiso 1 8 d S 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
I IA 0.56(3) . ?
I I 0.91(5) 28 ?
I I 0.91(5) 74 ?
I I 0.91(5) 51 ?

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
IA I I 35.265(2) . 28 ?
IA I I 35.265(2) . 74 ?
I I I 60.001(2) 28 74 ?
IA I I 35.265(1) . 51 ?
I I I 60.001(1) 28 51 ?
I I I 60.001(2) 74 51 ?
I IA I 109.471(8) . 28 ?
I IA I 109.471(9) . 74 ?
I IA I 109.471(17) 28 74 ?
I IA I 109.471(4) . 51 ?
I IA I 109.471(5) 28 51 ?
I IA I 109.47(2) 74 51 ?

_refine_diff_density_max         2.820
_refine_diff_density_min         -2.307
_refine_diff_density_rms         0.388



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Methylamine'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Hygroscopic
