# Electronic Supplementary Material (ESI) for Chemical Science.
# 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_I
_database_code_depnum_ccdc_archive 'CCDC 2018080'
loop_
_audit_author_name
_audit_author_address
'Justin Hoffman'
;Northwestern University
United States of America
;
_audit_update_record             
;
2020-07-21 deposited with the CCDC.	2020-10-06 downloaded from the CCDC.
;
#=======================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic        
; ?
;
_chemical_name_common            ?
_chemical_formula_moiety         '2(C5 H14 N 1+), 2(C H6 N 1+), Pb3 I10 4-'
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_iupac          ?
_chemical_formula_sum            'C12 H40 I10 N4 Pb3'
_chemical_formula_weight         2131.1
_chemical_melting_point          ?
_chemical_compound_source        ?
_chemical_absolute_configuration .

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

# 6. CRYSTAL DATA

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_Int_Tables_number      15

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

_cell_length_a                   8.9061(4)
_cell_length_b                   55.6891(5)
_cell_length_c                   8.9027(5)
_cell_angle_alpha                90.000
_cell_angle_beta                 90.055(4)
_cell_angle_gamma                90
_cell_volume                     4415.5(16)

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
? ? ? ? ? ? ? ? ? ? ?

_cell_formula_units_Z            4

_cell_measurement_reflns_used    5778
_cell_measurement_theta_min      1.46
_cell_measurement_theta_max      28.63
_cell_measurement_temperature    293
_cell_special_details            
; ?
;

_exptl_crystal_density_diffrn    3.2058
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             3664

_exptl_absorpt_coefficient_mu    18.412
_exptl_crystal_description       plate
_exptl_crystal_size_max          0.1122
_exptl_crystal_size_mid          0.801
_exptl_crystal_size_min          0.0425
_exptl_crystal_size_rad          ?
_exptl_crystal_colour            'dark red'
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   ?
_exptl_absorpt_correction_T_min  0.0592
_exptl_absorpt_correction_T_max  0.2349
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
30 -11 -1 0.1030
25 -8 30 0.1032
1 -15 -2 0.0787
2 30 -3 0.0814
0 1 0 0.0425
-1 -27 30 0.0904
0 -15 1 0.0630
-6 1 0 0.1094
-13 7 -15 0.1045
-1 10 0 0.0729
-24 23 30 0.1122
-1 -15 2 0.0771
0 -1 0 0.0456
0 -15 -1 0.0622
1 23 -30 0.1019
0 15 -1 0.0657

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

# 7. EXPERIMENTAL DATA

_exptl_special_details           ?

_diffrn_ambient_temperature      293
_diffrn_source                   ?
_diffrn_source_power             ?
_diffrn_source_voltage           ?
_diffrn_source_current           ?
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'IPDS Stoe'
_diffrn_detector                 ?
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_method       '??integration method??'
_diffrn_measurement_specimen_support ?

_diffrn_reflns_number            23303
_diffrn_reflns_theta_min         1.46
_diffrn_reflns_theta_max         29.24
_diffrn_reflns_theta_full        29.24
_diffrn_measured_fraction_theta_max 0.98
_diffrn_measured_fraction_theta_full 0.98
_diffrn_reflns_av_R_equivalents  0.1334
_diffrn_reflns_av_unetI/netI     0.1411
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -74
_diffrn_reflns_limit_k_max       76
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_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          
; The structure was refined based on the following considerations.
 The perovskite lattice was refined anisotropically without
 any constraints on the Pb and I atoms. The highly anisotropic shape of
 the thermal ellipsoids of coordinated iodide ions appears due to a high
 thermal motion relative to the Pb-I bond vector. It is typical for the
 halide perovskites structures at room temperature and therefore no 
 special treatment was used. All organic atoms were refined isotropically.
 Restraints were applied to the C-C and C-N bond lengths. Each cation was
 treated as having equivalent thermal parameters. Significant disorder 
 exists in the interlayer cations,  causing the atoms to move and destabilize the refinement. 
 The bond length restraints cannot account for the motion of the interlayer cations. 
 Therefore the cations were modeled manually based on reasonable
 bond length and bond angle parameters. Some of these cations are shown
 unreasonably close to one another due to this disorder.
;

_reflns_number_total             4003
_reflns_number_gt                1219
_reflns_threshold_expression     I>3σ(I)

_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_gt           0.0997
_refine_ls_wR_factor_gt          0.1892
_refine_ls_R_factor_all          0.2075
_refine_ls_wR_factor_ref         0.1958
_refine_ls_goodness_of_fit_ref   2.32
_refine_ls_goodness_of_fit_gt    4.17
_refine_ls_restrained_S_gt       ?
_refine_ls_restrained_S_all      ?
_refine_ls_number_reflns         4003
_refine_ls_number_parameters     90
_refine_ls_number_restraints     11
_refine_ls_number_constraints    86
_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          0.0451
_refine_ls_shift/su_mean         0.0030
_refine_diff_density_max         5.91
_refine_diff_density_min         -7.14
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_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 0.0033 0.0016 '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 -0.4742 1.8119 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
N 0.0061 0.0033 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
Pb -3.3944 10.1111 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  ?
_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
N1 . C1a . 1.5 0.001
C1a . C1b . 1.5 0.001
C1b . C1c . 1.5 0.001
C1c . C1d . 1.5 0.001
C1c . C1e . 1.5 0.001
N2 . C2 . 1.5 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
N1 . C1a . C1b . 109.47 0.01
C1a . C1b . C1c . 109.47 0.01
C1b . C1c . C1d . 109.47 0.01
C1b . C1c . C1e . 109.47 0.01
C1d . C1c . C1e . 109.47 0.01

loop_
_restr_torsion_atom_site_label_1
_restr_torsion_site_symmetry_1
_restr_torsion_atom_site_label_2
_restr_torsion_site_symmetry_2
_restr_torsion_atom_site_label_3
_restr_torsion_site_symmetry_3
_restr_torsion_atom_site_label_4
_restr_torsion_site_symmetry_4
_restr_torsion_angle_target
_restr_torsion_weight_param
? ? ? ? ? ? ? ? ? ?

loop_
_restr_equal_distance_atom_site_label_1
_restr_equal_distance_site_symmetry_1
_restr_equal_distance_atom_site_label_2
_restr_equal_distance_site_symmetry_2
_restr_equal_distance_class_class_id
_restr_equal_distance_class_target_weight_param
? ? ? ? ? ?

loop_
_restr_equal_angle_atom_site_label_1
_restr_equal_angle_site_symmetry_1
_restr_equal_angle_atom_site_label_2
_restr_equal_angle_site_symmetry_2
_restr_equal_angle_atom_site_label_3
_restr_equal_angle_site_symmetry_3
_restr_equal_angle_class_class_id
_restr_equal_angle_class_target_weight_param
? ? ? ? ? ? ? ?

loop_
_restr_equal_torsion_atom_site_label_1
_restr_equal_torsion_site_symmetry_1
_restr_equal_torsion_atom_site_label_2
_restr_equal_torsion_site_symmetry_2
_restr_equal_torsion_atom_site_label_3
_restr_equal_torsion_site_symmetry_3
_restr_equal_torsion_atom_site_label_4
_restr_equal_torsion_site_symmetry_4
_restr_equal_torsion_class_class_id
_restr_equal_torsion_class_target_weight_param
? ? ? ? ? ? ? ? ? ?


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

# 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 0.75 0.25 0 Uani 0.0603(8) 4 1 d . . .
Pb2 Pb 0.7512(3) 0.13385(2) 0.0012(3) Uani 0.0563(5) 8 1 d . . .
I1 I 0.5 0.13365(14) 0.25 Uani 0.151(4) 4 1 d . . .
I2 I 0 0.13326(14) 0.25 Uani 0.144(4) 4 1 d . . .
I3 I 0.7547(7) 0.19334(5) 0.0194(5) Uani 0.1050(13) 8 1 d . . .
I4 I 0.5 0.36123(12) 0.25 Uani 0.126(4) 4 1 d . . .
I5 I 0 0.36096(13) 0.25 Uani 0.126(4) 4 1 d . . .
I6 I 0.7428(9) 0.42027(7) 0.0327(6) Uani 0.180(3) 8 1 d . . .
I7 I 0 0.2503(2) 0.25 Uani 0.261(4) 4 1 d . . .
I8 I 0.5 0.25183(18) 0.25 Uani 0.266(4) 4 1 d . . .
N1 N 0.794(7) 0.3990(9) -0.509(8) Uiso 0.36(2) 8 1 d . . .
C1a C 0.722(6) 0.4211(10) -0.444(7) Uiso 0.36(2) 8 1 d . . .
C1b C 0.835(7) 0.4410(9) -0.438(7) Uiso 0.36(2) 8 1 d . . .
C1c C 0.772(6) 0.4629(9) -0.514(4) Uiso 0.36(2) 8 1 d . . .
N2 N -0.209(7) 0.3080(14) 0.457(6) Uiso 0.27(2) 8 1 d . . .
C2 C -0.222(10) 0.3035(11) 0.623(6) Uiso 0.27(2) 8 1 d . . .
C1d C 0.853(8) 0.4848(9) -0.459(8) Uiso 0.36(2) 8 1 d . . .
C1e C 0.608(6) 0.4651(13) -0.478(7) Uiso 0.36(2) 8 1 d . . .
H1c1a H 0.686575 0.417612 -0.344594 Uiso 0.4362 8 1 d . . .
H2c1a H 0.639034 0.425807 -0.506252 Uiso 0.4362 8 1 d . . .
H1c1b H 0.856973 0.444736 -0.334594 Uiso 0.4362 8 1 d . . .
H2c1b H 0.925198 0.436135 -0.487679 Uiso 0.4362 8 1 d . . .
H1c1c H 0.784444 0.461376 -0.620347 Uiso 0.4362 8 1 d . . .
H1c2 H -0.26043 0.287613 0.639406 Uiso 0.3197 8 1 d . . .
H2c2 H -0.12451 0.304886 0.668594 Uiso 0.3197 8 1 d . . .
H3c2 H -0.288617 0.315062 0.666389 Uiso 0.3197 8 1 d . . .
H1c1d H 0.818672 0.488838 -0.360244 Uiso 0.4362 8 1 d . . .
H2c1d H 0.959124 0.481605 -0.456123 Uiso 0.4362 8 1 d . . .
H3c1d H 0.8339 0.497925 -0.526196 Uiso 0.4362 8 1 d . . .
H1c1e H 0.553278 0.468928 -0.567332 Uiso 0.4362 8 1 d . . .
H2c1e H 0.572027 0.450139 -0.437537 Uiso 0.4362 8 1 d . . .
H3c1e H 0.593802 0.477576 -0.404697 Uiso 0.4362 8 1 d . . .
H1n1 H 0.728572 0.387504 -0.51347 Uiso 0.4362 8 1 d . . .
H2n1 H 0.827054 0.402209 -0.598808 Uiso 0.4362 8 1 d . . .
H3n1 H 0.868931 0.394672 -0.452179 Uiso 0.4362 8 1 d . . .
H1n2 H -0.295621 0.312376 0.421843 Uiso 0.3197 8 1 d . . .
H2n2 H -0.143309 0.319301 0.441316 Uiso 0.3197 8 1 d . . .
H3n2 H -0.179813 0.294898 0.412437 Uiso 0.3197 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 I3 . . 3.160(3) ?
Pb1 I3 . 7_655 3.160(3) ?
Pb1 I7 . 1_655 3.1467(11) ?
Pb1 I7 . 7_555 3.1467(11) ?
Pb1 I8 . . 3.1513(12) ?
Pb1 I8 . 7_655 3.1513(12) ?
Pb2 I1 . . 3.150(3) ?
Pb2 I2 . 1_655 3.132(3) ?
Pb2 I3 . . 3.317(3) ?
Pb2 I4 . 7_655 3.161(3) ?
Pb2 I5 . 7_555 3.175(3) ?
Pb2 I6 . 7_655 3.030(4) ?
I1 N1 . 7_655 3.46(7) ?
I1 N1 . 8_455 3.46(7) ?
I5 N1 . 1_456 3.53(6) ?
I5 N1 . 2_654 3.53(6) ?
N1 C1a . . 1.50(8) ?
N1 H1n1 . . 0.87 ?
N1 H2n1 . . 0.87 ?
N1 H3n1 . . 0.87 ?
C1a C1b . . 1.50(8) ?
C1a H1c1a . . 0.96 ?
C1a H2c1a . . 0.96 ?
C1b C1c . . 1.50(7) ?
C1b H1c1b . . 0.96 ?
C1b H2c1b . . 0.96 ?
C1c C1d . . 1.50(8) ?
C1c C1e . . 1.50(8) ?
C1c H1c1c . . 0.96 ?
N2 C2 . . 1.50(7) ?
N2 H1n2 . . 0.87 ?
N2 H2n2 . . 0.87 ?
N2 H3n2 . . 0.87 ?
C2 H1c2 . . 0.96 ?
C2 H2c2 . . 0.96 ?
C2 H3c2 . . 0.96 ?
C1d H1c1d . . 0.96 ?
C1d H2c1d . . 0.96 ?
C1d H3c1d . . 0.96 ?
C1e H1c1e . . 0.96 ?
C1e H2c1e . . 0.96 ?
C1e H3c1e . . 0.96 ?

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
I3 Pb1 I3 . . 7_655 180.0(5) ?
I3 Pb1 I7 . . 1_655 87.6(2) ?
I3 Pb1 I7 . . 7_555 92.4(2) ?
I3 Pb1 I8 . . . 90.2(2) ?
I3 Pb1 I8 . . 7_655 89.8(2) ?
I3 Pb1 I7 7_655 . 1_655 92.4(2) ?
I3 Pb1 I7 7_655 . 7_555 87.6(2) ?
I3 Pb1 I8 7_655 . . 89.8(2) ?
I3 Pb1 I8 7_655 . 7_655 90.2(2) ?
I7 Pb1 I7 1_655 . 7_555 180.0(5) ?
I7 Pb1 I8 1_655 . . 90.01(2) ?
I7 Pb1 I8 1_655 . 7_655 89.99(2) ?
I7 Pb1 I8 7_555 . . 89.99(2) ?
I7 Pb1 I8 7_555 . 7_655 90.01(2) ?
I8 Pb1 I8 . . 7_655 180.0(5) ?
I1 Pb2 I2 . . 1_655 90.29(7) ?
I1 Pb2 I3 . . . 88.62(18) ?
I1 Pb2 I4 . . 7_655 175.2(2) ?
I1 Pb2 I5 . . 7_555 89.72(8) ?
I1 Pb2 I6 . . 7_655 94.5(2) ?
I2 Pb2 I3 1_655 . . 88.24(18) ?
I2 Pb2 I4 1_655 . 7_655 90.31(8) ?
I2 Pb2 I5 1_655 . 7_555 175.4(2) ?
I2 Pb2 I6 1_655 . 7_655 92.7(2) ?
I3 Pb2 I4 . . 7_655 86.64(16) ?
I3 Pb2 I5 . . 7_555 87.14(16) ?
I3 Pb2 I6 . . 7_655 176.70(17) ?
I4 Pb2 I5 7_655 . 7_555 89.31(7) ?
I4 Pb2 I6 7_655 . 7_655 90.19(19) ?
I5 Pb2 I6 7_555 . 7_655 91.90(19) ?
Pb2 I1 Pb2 . . 2_655 179.6(3) ?
Pb2 I1 N1 . . 7_655 95.4(11) ?
Pb2 I1 N1 . . 8_455 84.8(11) ?
Pb2 I1 N1 2_655 . 7_655 84.8(11) ?
Pb2 I1 N1 2_655 . 8_455 95.4(11) ?
N1 I1 N1 7_655 . 8_455 116.5(14) ?
Pb2 I2 Pb2 1_455 . 2_655 178.8(3) ?
Pb1 I3 Pb2 . . . 173.93(15) ?
Pb2 I4 Pb2 7_655 . 8_455 170.1(2) ?
Pb2 I5 Pb2 7_555 . 8_455 169.6(3) ?
Pb2 I5 N1 7_555 . 1_456 90.4(11) ?
Pb2 I5 N1 7_555 . 2_654 83.3(11) ?
Pb2 I5 N1 8_455 . 1_456 83.3(11) ?
Pb2 I5 N1 8_455 . 2_654 90.4(11) ?
N1 I5 N1 1_456 . 2_654 106.2(14) ?
Pb1 I7 Pb1 1_455 . 2_655 179.3(4) ?
Pb1 I8 Pb1 . . 2_655 176.3(4) ?
I1 N1 I5 7_655 . 1_654 79.3(12) ?
I1 N1 C1a 7_655 . . 114(4) ?
I1 N1 H1n1 7_655 . . 89.85 ?
I1 N1 H2n1 7_655 . . 122.73 ?
I1 N1 H3n1 7_655 . . 20.21 ?
I5 N1 C1a 1_654 . . 161(4) ?
I5 N1 H1n1 1_654 . . 82.94 ?
I5 N1 H2n1 1_654 . . 52.24 ?
I5 N1 H3n1 1_654 . . 77.74 ?
C1a N1 H1n1 . . . 109.47 ?
C1a N1 H2n1 . . . 109.47 ?
C1a N1 H3n1 . . . 109.47 ?
H1n1 N1 H2n1 . . . 109.47 ?
H1n1 N1 H3n1 . . . 109.47 ?
H2n1 N1 H3n1 . . . 109.47 ?
N1 C1a C1b . . . 109(5) ?
N1 C1a H1c1a . . . 109.47 ?
N1 C1a H2c1a . . . 109.47 ?
C1b C1a H1c1a . . . 109.47 ?
C1b C1a H2c1a . . . 109.47 ?
H1c1a C1a H2c1a . . . 109.47 ?
C1a C1b C1c . . . 109(5) ?
C1a C1b H1c1b . . . 109.47 ?
C1a C1b H2c1b . . . 109.47 ?
C1c C1b H1c1b . . . 109.47 ?
C1c C1b H2c1b . . . 109.47 ?
H1c1b C1b H2c1b . . . 109.47 ?
C1b C1c C1d . . . 109(4) ?
C1b C1c C1e . . . 109(5) ?
C1b C1c H1c1c . . . 109.48 ?
C1d C1c C1e . . . 109(5) ?
C1d C1c H1c1c . . . 109.47 ?
C1e C1c H1c1c . . . 109.47 ?
C2 N2 H1n2 . . . 109.47 ?
C2 N2 H2n2 . . . 109.47 ?
C2 N2 H3n2 . . . 109.47 ?
H1n2 N2 H2n2 . . . 109.47 ?
H1n2 N2 H3n2 . . . 109.47 ?
H2n2 N2 H3n2 . . . 109.47 ?
N2 C2 H1c2 . . . 109.47 ?
N2 C2 H2c2 . . . 109.47 ?
N2 C2 H3c2 . . . 109.47 ?
H1c2 C2 H2c2 . . . 109.47 ?
H1c2 C2 H3c2 . . . 109.47 ?
H2c2 C2 H3c2 . . . 109.47 ?
C1c C1d H1c1d . . . 109.47 ?
C1c C1d H2c1d . . . 109.47 ?
C1c C1d H3c1d . . . 109.47 ?
H1c1d C1d H2c1d . . . 109.47 ?
H1c1d C1d H3c1d . . . 109.47 ?
H2c1d C1d H3c1d . . . 109.47 ?
C1c C1e H1c1e . . . 109.47 ?
C1c C1e H2c1e . . . 109.47 ?
C1c C1e H3c1e . . . 109.47 ?
H1c1e C1e H2c1e . . . 109.47 ?
H1c1e C1e H3c1e . . . 109.47 ?
H2c1e C1e H3c1e . . . 109.47 ?

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
C1a H2c1a C1e . . . 0.96 2.22 2.67(9) 107.52 ?
C1e H2c1e C1a . . . 0.96 2.10 2.67(9) 116.44 ?


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Hydriodic Acid'
####################################################################### 
# 
# 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_I_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2018086'
loop_
_audit_author_name
_audit_author_address
'Justin Hoffman'
;Northwestern University
United States of America
;
_audit_update_record             
;
2020-07-21 deposited with the CCDC.	2020-10-06 downloaded from the CCDC.
;
#=======================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic        
; ?
;
_chemical_name_common            ?
_chemical_formula_moiety         '2(C4 H12 N 1+), Pb I4 2-'
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_iupac          ?
_chemical_formula_sum            'C8 H24 I4 N2 Pb1'
_chemical_formula_weight         863.1
_chemical_melting_point          ?
_chemical_compound_source        ?
_chemical_absolute_configuration .

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

# 6. CRYSTAL DATA

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ycb'
_symmetry_Int_Tables_number      14

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,-z
4 x,-y+1/2,z+1/2

_cell_length_a                   13.8298(7)
_cell_length_b                   8.9872(3)
_cell_length_c                   8.7822(3)
_cell_angle_alpha                90
_cell_angle_beta                 108.213(5)
_cell_angle_gamma                90
_cell_volume                     1036.86(8)

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
? ? ? ? ? ? ? ? ? ? ?

_cell_formula_units_Z            2

_cell_measurement_reflns_used    8363
_cell_measurement_theta_min      2.72
_cell_measurement_theta_max      29.55
_cell_measurement_temperature    288(5)
_cell_special_details            
; ?
;

_exptl_crystal_density_diffrn    2.7645
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             760

_exptl_absorpt_coefficient_mu    14.074
_exptl_crystal_description       plate
_exptl_crystal_size_max          0.188
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.027
_exptl_crystal_size_rad          ?
_exptl_crystal_colour            orange
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.25a (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.202
_exptl_absorpt_correction_T_max  0.839
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      288
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_power             ?
_diffrn_source_voltage           ?
_diffrn_source_current           ?
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       ?
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support ?

_diffrn_reflns_number            12785
_diffrn_reflns_theta_min         2.75
_diffrn_reflns_theta_max         29.59
_diffrn_reflns_theta_full        29.59
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measured_fraction_theta_full 0.99
_diffrn_reflns_av_R_equivalents  0.05
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       12
_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             1875
_reflns_number_gt                1693
_reflns_threshold_expression     I>3σ(I)

_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_gt           0.0342
_refine_ls_wR_factor_gt          0.0911
_refine_ls_R_factor_all          0.0366
_refine_ls_wR_factor_ref         0.0917
_refine_ls_goodness_of_fit_ref   2.40
_refine_ls_goodness_of_fit_gt    2.51
_refine_ls_restrained_S_gt       ?
_refine_ls_restrained_S_all      ?
_refine_ls_number_reflns         1875
_refine_ls_number_parameters     41
_refine_ls_number_restraints     8
_refine_ls_number_constraints    52
_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          0.0459
_refine_ls_shift/su_mean         0.0032
_refine_diff_density_max         1.61
_refine_diff_density_min         -1.60
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_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 0.0033 0.0016 '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 -0.4742 1.8119 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
N 0.0061 0.0033 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
Pb -3.3944 10.1111 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'

_computing_data_collection       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_structure_solution    ?
_computing_structure_refinement  ?
_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
N1 . C1a . 1.5 0.001
C1a . C1b . 1.5 0.001
C1b . C1c . 1.5 0.001
C1b . C1d . 1.5 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
N1 . C1a . C1b . 109.47 0.01
C1a . C1b . C1c . 109.47 0.01
C1a . C1b . C1d . 109.47 0.01
C1c . C1b . C1d . 109.47 0.01

loop_
_restr_torsion_atom_site_label_1
_restr_torsion_site_symmetry_1
_restr_torsion_atom_site_label_2
_restr_torsion_site_symmetry_2
_restr_torsion_atom_site_label_3
_restr_torsion_site_symmetry_3
_restr_torsion_atom_site_label_4
_restr_torsion_site_symmetry_4
_restr_torsion_angle_target
_restr_torsion_weight_param
? ? ? ? ? ? ? ? ? ?

loop_
_restr_equal_distance_atom_site_label_1
_restr_equal_distance_site_symmetry_1
_restr_equal_distance_atom_site_label_2
_restr_equal_distance_site_symmetry_2
_restr_equal_distance_class_class_id
_restr_equal_distance_class_target_weight_param
? ? ? ? ? ?

loop_
_restr_equal_angle_atom_site_label_1
_restr_equal_angle_site_symmetry_1
_restr_equal_angle_atom_site_label_2
_restr_equal_angle_site_symmetry_2
_restr_equal_angle_atom_site_label_3
_restr_equal_angle_site_symmetry_3
_restr_equal_angle_class_class_id
_restr_equal_angle_class_target_weight_param
? ? ? ? ? ? ? ?

loop_
_restr_equal_torsion_atom_site_label_1
_restr_equal_torsion_site_symmetry_1
_restr_equal_torsion_atom_site_label_2
_restr_equal_torsion_site_symmetry_2
_restr_equal_torsion_atom_site_label_3
_restr_equal_torsion_site_symmetry_3
_restr_equal_torsion_atom_site_label_4
_restr_equal_torsion_site_symmetry_4
_restr_equal_torsion_class_class_id
_restr_equal_torsion_class_target_weight_param
? ? ? ? ? ? ? ? ? ?


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

# 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 0.5 0.5 0 Uani 0.03730(17) 2 1 d . . .
I1 I 0.48992(5) 0.19978(6) 0.19329(6) Uani 0.0522(2) 4 1 d . . .
I2 I 0.74184(5) 0.46303(8) 0.13515(8) Uani 0.0610(3) 4 1 d . . .
N1 N 0.7003(7) 0.0751(11) 0.0256(11) Uiso 0.1062(19) 4 1 d . . .
C1a C 0.7463(6) -0.0440(10) 0.1462(12) Uiso 0.1062(19) 4 1 d . . .
C1b C 0.8562(6) -0.0085(7) 0.2291(9) Uiso 0.1062(19) 4 1 d . . .
C1c C 0.9036(8) -0.1315(13) 0.3437(12) Uiso 0.1062(19) 4 1 d . . .
C1d C 0.9110(8) 0.0064(14) 0.1070(13) Uiso 0.1062(19) 4 1 d . . .
H1c1a H 0.710563 -0.048593 0.223831 Uiso 0.1275 4 1 d . . .
H2c1a H 0.741183 -0.138175 0.092744 Uiso 0.1275 4 1 d . . .
H1c1b H 0.86121 0.083238 0.286994 Uiso 0.1275 4 1 d . . .
H1c1c H 0.856514 -0.164471 0.39691 Uiso 0.1275 4 1 d . . .
H2c1c H 0.920251 -0.212991 0.285772 Uiso 0.1275 4 1 d . . .
H3c1c H 0.964495 -0.09556 0.421754 Uiso 0.1275 4 1 d . . .
H1c1d H 0.958701 0.087064 0.136388 Uiso 0.1275 4 1 d . . .
H2c1d H 0.946641 -0.084325 0.102574 Uiso 0.1275 4 1 d . . .
H3c1d H 0.862579 0.026008 0.003719 Uiso 0.1275 4 1 d . . .
H1n1 H 0.650203 0.03776 -0.051468 Uiso 0.1275 4 1 d . . .
H2n1 H 0.677662 0.146728 0.07181 Uiso 0.1275 4 1 d . . .
H3n1 H 0.746277 0.109751 -0.013596 Uiso 0.1275 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 . . 3.2139(6) ?
Pb1 I1 . 2_655 3.2037(6) ?
Pb1 I1 . 3_665 3.2139(6) ?
Pb1 I1 . 4_554 3.2037(6) ?
Pb1 I2 . . 3.1975(7) ?
Pb1 I2 . 3_665 3.1975(7) ?
I1 N1 . . 3.817(11) ?
I1 N1 . 3_655 3.682(9) ?
I2 N1 . . 3.615(10) ?
I2 N1 . 4_555 3.665(11) ?
N1 C1a . . 1.500(13) ?
N1 H1n1 . . 0.87 ?
N1 H2n1 . . 0.87 ?
N1 H3n1 . . 0.87 ?
C1a C1b . . 1.500(10) ?
C1a H1c1a . . 0.96 ?
C1a H2c1a . . 0.96 ?
C1b C1c . . 1.500(12) ?
C1b C1d . . 1.500(16) ?
C1b H1c1b . . 0.96 ?
C1c H1c1c . . 0.96 ?
C1c H2c1c . . 0.96 ?
C1c H3c1c . . 0.96 ?
C1d H1c1d . . 0.96 ?
C1d H2c1d . . 0.96 ?
C1d H3c1d . . 0.96 ?

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 . . 2_655 91.380(14) ?
I1 Pb1 I1 . . 3_665 180.0(5) ?
I1 Pb1 I1 . . 4_554 88.620(14) ?
I1 Pb1 I2 . . . 85.969(17) ?
I1 Pb1 I2 . . 3_665 94.031(17) ?
I1 Pb1 I1 2_655 . 3_665 88.620(14) ?
I1 Pb1 I1 2_655 . 4_554 180.0(5) ?
I1 Pb1 I2 2_655 . . 88.886(17) ?
I1 Pb1 I2 2_655 . 3_665 91.114(17) ?
I1 Pb1 I1 3_665 . 4_554 91.380(14) ?
I1 Pb1 I2 3_665 . . 94.031(17) ?
I1 Pb1 I2 3_665 . 3_665 85.969(17) ?
I1 Pb1 I2 4_554 . . 91.114(17) ?
I1 Pb1 I2 4_554 . 3_665 88.886(17) ?
I2 Pb1 I2 . . 3_665 180.0(5) ?
Pb1 I1 Pb1 . . 2_645 156.477(18) ?
Pb1 I1 N1 . . . 83.03(15) ?
Pb1 I1 N1 . . 3_655 115.43(15) ?
Pb1 I1 N1 2_645 . . 108.77(14) ?
Pb1 I1 N1 2_645 . 3_655 84.21(16) ?
N1 I1 N1 . . 3_655 96.2(2) ?
Pb1 I2 N1 . . . 86.59(15) ?
Pb1 I2 N1 . . 4_555 84.57(14) ?
N1 I2 N1 . . 4_555 95.8(2) ?
I1 N1 I1 . . 3_655 83.8(2) ?
I1 N1 I2 . . . 72.00(19) ?
I1 N1 I2 . . 4_554 138.6(2) ?
I1 N1 C1a . . . 98.2(6) ?
I1 N1 H1n1 . . . 84.02 ?
I1 N1 H2n1 . . . 34.3 ?
I1 N1 H3n1 . . . 141.91 ?
I1 N1 I2 3_655 . . 144.5(3) ?
I1 N1 I2 3_655 . 4_554 75.19(18) ?
I1 N1 C1a 3_655 . . 88.1(5) ?
I1 N1 H1n1 3_655 . . 21.6 ?
I1 N1 H2n1 3_655 . . 115.97 ?
I1 N1 H3n1 3_655 . . 121.69 ?
I2 N1 I2 . . 4_554 106.3(3) ?
I2 N1 C1a . . . 120.2(6) ?
I2 N1 H1n1 . . . 126.9 ?
I2 N1 H2n1 . . . 38.02 ?
I2 N1 H3n1 . . . 71.62 ?
I2 N1 C1a 4_554 . . 116.0(7) ?
I2 N1 H1n1 4_554 . . 63.64 ?
I2 N1 H2n1 4_554 . . 133.64 ?
I2 N1 H3n1 4_554 . . 46.83 ?
C1a N1 H1n1 . . . 109.47 ?
C1a N1 H2n1 . . . 109.47 ?
C1a N1 H3n1 . . . 109.47 ?
H1n1 N1 H2n1 . . . 109.47 ?
H1n1 N1 H3n1 . . . 109.47 ?
H2n1 N1 H3n1 . . . 109.47 ?
N1 C1a C1b . . . 109.5(7) ?
N1 C1a H1c1a . . . 109.47 ?
N1 C1a H2c1a . . . 109.47 ?
C1b C1a H1c1a . . . 109.47 ?
C1b C1a H2c1a . . . 109.47 ?
H1c1a C1a H2c1a . . . 109.47 ?
C1a C1b C1c . . . 109.5(7) ?
C1a C1b C1d . . . 109.5(7) ?
C1a C1b H1c1b . . . 109.47 ?
C1c C1b C1d . . . 109.5(8) ?
C1c C1b H1c1b . . . 109.47 ?
C1d C1b H1c1b . . . 109.47 ?
C1b C1c H1c1c . . . 109.47 ?
C1b C1c H2c1c . . . 109.47 ?
C1b C1c H3c1c . . . 109.47 ?
H1c1c C1c H2c1c . . . 109.47 ?
H1c1c C1c H3c1c . . . 109.47 ?
H2c1c C1c H3c1c . . . 109.47 ?
C1b C1d H1c1d . . . 109.47 ?
C1b C1d H2c1d . . . 109.47 ?
C1b C1d H3c1d . . . 109.47 ?
H1c1d C1d H2c1d . . . 109.47 ?
H1c1d C1d H3c1d . . . 109.47 ?
H2c1d C1d H3c1d . . . 109.47 ?

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
C1d H3c1d N1 . . . 0.96 2.35 2.842(14) 111.00 ?
N1 H3n1 C1d . . . 0.87 2.38 2.842(14) 113.62 ?


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Hydriodic Acid'
####################################################################### 
# 
# 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_I_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 2018082'
loop_
_audit_author_name
_audit_author_address
'Justin Hoffman'
;Northwestern University
United States of America
;
_audit_update_record             
;
2020-07-21 deposited with the CCDC.	2020-10-06 downloaded from the CCDC.
;
#=======================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic        
; ?
;
_chemical_name_common            ?
_chemical_formula_moiety         '2(C4 H12 N 1+), 2(C H6 N 1+), Pb3 I10 4-'
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_iupac          ?
_chemical_formula_sum            'C11 H36 I10 N4 Pb3'
_chemical_formula_weight         2115.1
_chemical_melting_point          ?
_chemical_compound_source        ?
_chemical_absolute_configuration .

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

# 6. CRYSTAL DATA

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_Int_Tables_number      15

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

_cell_length_a                   8.9429(6)
_cell_length_b                   8.9415(4)
_cell_length_c                   51.048(3)
_cell_angle_alpha                90.000
_cell_angle_beta                 90.006(5)
_cell_angle_gamma                90
_cell_volume                     4082.0(16)

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
? ? ? ? ? ? ? ? ? ? ?

_cell_formula_units_Z            4

_cell_measurement_reflns_used    34185
_cell_measurement_theta_min      2.28
_cell_measurement_theta_max      29.24
_cell_measurement_temperature    293
_cell_special_details            
; ?
;

_exptl_crystal_density_diffrn    3.4416
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             3600

_exptl_absorpt_coefficient_mu    19.915
_exptl_crystal_description       plate
_exptl_crystal_size_max          0.1031
_exptl_crystal_size_mid          0.0884
_exptl_crystal_size_min          0.0341
_exptl_crystal_size_rad          ?
_exptl_crystal_colour            'dark red'
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   ?
_exptl_absorpt_correction_T_min  0.0526
_exptl_absorpt_correction_T_max  0.2556
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
15 -1 6 0.0887
30 -22 -1 0.0893
1 1 -10 0.0491
0 30 -11 0.0884
0 0 1 0.0341
-1 0 0 0.1031
-28 -30 -1 0.0863
-1 -1 -10 0.0572
-30 29 4 0.0937
2 -15 -2 0.1006
0 0 -1 0.0459

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

# 7. EXPERIMENTAL DATA

_exptl_special_details           ?

_diffrn_ambient_temperature      293
_diffrn_source                   ?
_diffrn_source_power             ?
_diffrn_source_voltage           ?
_diffrn_source_current           ?
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'IPDS Stoe'
_diffrn_detector                 ?
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_method       '??integration method??'
_diffrn_measurement_specimen_support ?

_diffrn_reflns_number            16563
_diffrn_reflns_theta_min         3.22
_diffrn_reflns_theta_max         29.22
_diffrn_reflns_theta_full        29.22
_diffrn_measured_fraction_theta_max 0.97
_diffrn_measured_fraction_theta_full 0.97
_diffrn_reflns_av_R_equivalents  0.2104
_diffrn_reflns_av_unetI/netI     0.1365
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -70
_diffrn_reflns_limit_l_max       68
_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          
; The structure was refined based on the following considerations.
 The perovskite lattice was refined anisotropically without
 any constraints on the Pb and I atoms. The highly anisotropic shape of
 the thermal ellipsoids of coordinated iodide ions appears due to a high
 thermal motion relative to the Pb-I bond vector. It is typical for the
 halide perovskites structures at room temperature and therefore no 
 special treatment was used. All organic atoms were refined isotropically.
 Restraints were applied to the C-C and C-N bond lengths. Each cation was
 treated as having equivalent thermal parameters. Significant disorder 
 exists in the interlayer cations,  causing the atoms to move and destabilize the refinement. 
 The bond length restraints cannot account for the motion of the interlayer cations. 
 Therefore the cations were modeled manually based on reasonable
 bond length and bond angle parameters. Some of these cations are shown
 unreasonably close to one another due to this disorder.
;

_reflns_number_total             3587
_reflns_number_gt                1119
_reflns_threshold_expression     I>3σ(I)

_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_gt           0.1190
_refine_ls_wR_factor_gt          0.2492
_refine_ls_R_factor_all          0.2317
_refine_ls_wR_factor_ref         0.2606
_refine_ls_goodness_of_fit_ref   3.57
_refine_ls_goodness_of_fit_gt    6.27
_refine_ls_restrained_S_gt       ?
_refine_ls_restrained_S_all      ?
_refine_ls_number_reflns         3587
_refine_ls_number_parameters     84
_refine_ls_number_restraints     9
_refine_ls_number_constraints    77
_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          0.0463
_refine_ls_shift/su_mean         0.0033
_refine_diff_density_max         3.98
_refine_diff_density_min         -4.84
_refine_ls_extinction_method     
'B-C type 1 Gaussian isotropic (Becker & Coppens, 1974)'
_refine_ls_extinction_coef       1180(130)
_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 0.0033 0.0016 '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 -0.4742 1.8119 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
N 0.0061 0.0033 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
Pb -3.3944 10.1111 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  ?
_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
N1 . C1a . 1.5 0.001
C1a . C1b . 1.5 0.001
C1b . C1c . 1.5 0.001
C1b . C1d . 1.5 0.001
N2 . C2 . 1.5 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
N1 . C1a . C1b . 109.47 0.01
C1a . C1b . C1c . 109.47 0.01
C1a . C1b . C1d . 109.47 0.01
C1c . C1b . C1d . 109.47 0.01

loop_
_restr_torsion_atom_site_label_1
_restr_torsion_site_symmetry_1
_restr_torsion_atom_site_label_2
_restr_torsion_site_symmetry_2
_restr_torsion_atom_site_label_3
_restr_torsion_site_symmetry_3
_restr_torsion_atom_site_label_4
_restr_torsion_site_symmetry_4
_restr_torsion_angle_target
_restr_torsion_weight_param
? ? ? ? ? ? ? ? ? ?

loop_
_restr_equal_distance_atom_site_label_1
_restr_equal_distance_site_symmetry_1
_restr_equal_distance_atom_site_label_2
_restr_equal_distance_site_symmetry_2
_restr_equal_distance_class_class_id
_restr_equal_distance_class_target_weight_param
? ? ? ? ? ?

loop_
_restr_equal_angle_atom_site_label_1
_restr_equal_angle_site_symmetry_1
_restr_equal_angle_atom_site_label_2
_restr_equal_angle_site_symmetry_2
_restr_equal_angle_atom_site_label_3
_restr_equal_angle_site_symmetry_3
_restr_equal_angle_class_class_id
_restr_equal_angle_class_target_weight_param
? ? ? ? ? ? ? ?

loop_
_restr_equal_torsion_atom_site_label_1
_restr_equal_torsion_site_symmetry_1
_restr_equal_torsion_atom_site_label_2
_restr_equal_torsion_site_symmetry_2
_restr_equal_torsion_atom_site_label_3
_restr_equal_torsion_site_symmetry_3
_restr_equal_torsion_atom_site_label_4
_restr_equal_torsion_site_symmetry_4
_restr_equal_torsion_class_class_id
_restr_equal_torsion_class_target_weight_param
? ? ? ? ? ? ? ? ? ?


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

# 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 0.00015(19) 0.2524(4) 0.12473(3) Uani 0.0516(8) 8 1 d . . .
Pb2 Pb 0 0.2526(7) 0.25 Uani 0.0481(10) 4 1 d . . .
I1 I 0.2592(8) 0.0057(11) 0.2501(3) Uani 0.141(3) 8 1 d . . .
I2 I 0.2584(5) 0.0025(7) 0.12624(17) Uani 0.137(5) 8 1 d . . .
I3 I 0.2408(6) 0.5031(8) 0.12597(19) Uani 0.144(6) 8 1 d . . .
I4 I -0.0003(7) 0.2629(14) 0.18873(10) Uani 0.178(3) 8 1 d . . .
I5 I -0.0025(10) 0.264(2) 0.06564(12) Uani 0.277(6) 8 1 d . . .
N1 N 0.472(8) 0.202(8) 0.0767(12) Uiso 0.27(2) 8 1 d . . .
C1a C 0.598(7) 0.150(8) 0.0596(16) Uiso 0.27(2) 8 1 d . . .
N2 N 0.108(6) 0.658(6) 0.1829(12) Uiso 0.16(2) 8 1 d . . .
C2 C -0.007(6) 0.762(8) 0.1939(13) Uiso 0.16(2) 8 1 d . . .
C1b C 0.566(6) 0.192(7) 0.0317(14) Uiso 0.27(2) 8 1 d . . .
C1c C 0.645(8) 0.335(9) 0.0252(17) Uiso 0.27(2) 8 1 d . . .
C1d C 0.401(6) 0.211(12) 0.0280(15) Uiso 0.27(2) 8 1 d . . .
H1c1a H 0.689265 0.197087 0.065156 Uiso 0.3297 8 1 d . . .
H2c1a H 0.607875 0.043644 0.060979 Uiso 0.3297 8 1 d . . .
H1c2 H -0.002554 0.855789 0.184854 Uiso 0.1893 8 1 d . . .
H2c2 H -0.104607 0.718829 0.191777 Uiso 0.1893 8 1 d . . .
H3c2 H 0.012072 0.777796 0.212238 Uiso 0.1893 8 1 d . . .
H1c1b H 0.601679 0.113995 0.020291 Uiso 0.3297 8 1 d . . .
H1c1c H 0.586628 0.418248 0.031472 Uiso 0.3297 8 1 d . . .
H2c1c H 0.741348 0.336572 0.033413 Uiso 0.3297 8 1 d . . .
H3c1c H 0.656599 0.343388 0.006556 Uiso 0.3297 8 1 d . . .
H1c1d H 0.367853 0.150153 0.013703 Uiso 0.3297 8 1 d . . .
H2c1d H 0.349975 0.182214 0.043731 Uiso 0.3297 8 1 d . . .
H3c1d H 0.379703 0.314403 0.024242 Uiso 0.3297 8 1 d . . .
H1n1 H 0.490986 0.291542 0.082477 Uiso 0.3297 8 1 d . . .
H2n1 H 0.389396 0.203801 0.067589 Uiso 0.3297 8 1 d . . .
H3n1 H 0.461575 0.141133 0.08982 Uiso 0.3297 8 1 d . . .
H1n2 H 0.065655 0.574883 0.178062 Uiso 0.1893 8 1 d . . .
H2n2 H 0.151456 0.699392 0.169521 Uiso 0.1893 8 1 d . . .
H3n2 H 0.175142 0.638403 0.194882 Uiso 0.1893 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 I2 . . 3.214(6) ?
Pb1 I2 . 5_455 3.111(7) ?
Pb1 I3 . . 3.108(7) ?
Pb1 I3 . 5_445 3.218(7) ?
Pb1 I4 . . 3.268(5) ?
Pb1 I5 . . 3.019(6) ?
Pb2 I1 . . 3.201(10) ?
Pb2 I1 . 5_455 3.124(10) ?
Pb2 I1 . 2_555 3.201(10) ?
Pb2 I1 . 6_555 3.124(10) ?
Pb2 I4 . . 3.129(5) ?
Pb2 I4 . 2_555 3.129(5) ?
I2 N1 . . 3.64(7) ?
I3 N2 . . 3.43(6) ?
I4 N2 . . 3.67(6) ?
I4 N2 . 5_445 3.64(5) ?
N1 C1a . . 1.50(10) ?
N1 H1n1 . . 0.87 ?
N1 H2n1 . . 0.87 ?
N1 H3n1 . . 0.87 ?
C1a C1b . . 1.50(11) ?
C1a H1c1a . . 0.96 ?
C1a H2c1a . . 0.96 ?
N2 C2 . . 1.50(8) ?
N2 H1n2 . . 0.87 ?
N2 H2n2 . . 0.87 ?
N2 H3n2 . . 0.87 ?
C2 H1c2 . . 0.96 ?
C2 H2c2 . . 0.96 ?
C2 H3c2 . . 0.96 ?
C1b C1c . . 1.50(10) ?
C1b C1d . . 1.50(8) ?
C1b H1c1b . . 0.96 ?
C1c H1c1c . . 0.96 ?
C1c H2c1c . . 0.96 ?
C1c H3c1c . . 0.96 ?
C1d H1c1d . . 0.96 ?
C1d H2c1d . . 0.96 ?
C1d H3c1d . . 0.96 ?

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
I2 Pb1 I2 . . 5_455 176.6(2) ?
I2 Pb1 I3 . . . 90.19(16) ?
I2 Pb1 I3 . . 5_445 92.05(18) ?
I2 Pb1 I4 . . . 89.8(2) ?
I2 Pb1 I5 . . . 93.1(3) ?
I2 Pb1 I3 5_455 . . 87.84(18) ?
I2 Pb1 I3 5_455 . 5_445 89.81(16) ?
I2 Pb1 I4 5_455 . . 87.4(2) ?
I2 Pb1 I5 5_455 . . 89.7(4) ?
I3 Pb1 I3 . . 5_445 176.8(2) ?
I3 Pb1 I4 . . . 87.7(3) ?
I3 Pb1 I5 . . . 90.0(4) ?
I3 Pb1 I4 5_445 . . 90.0(2) ?
I3 Pb1 I5 5_445 . . 92.2(3) ?
I4 Pb1 I5 . . . 176.3(5) ?
I1 Pb2 I1 . . 5_455 177.2(3) ?
I1 Pb2 I1 . . 2_555 92.8(3) ?
I1 Pb2 I1 . . 6_555 90.0(2) ?
I1 Pb2 I4 . . . 91.3(3) ?
I1 Pb2 I4 . . 2_555 91.0(3) ?
I1 Pb2 I1 5_455 . 2_555 90.0(2) ?
I1 Pb2 I1 5_455 . 6_555 87.2(3) ?
I1 Pb2 I4 5_455 . . 88.9(3) ?
I1 Pb2 I4 5_455 . 2_555 88.7(3) ?
I1 Pb2 I1 2_555 . 6_555 177.2(3) ?
I1 Pb2 I4 2_555 . . 91.0(3) ?
I1 Pb2 I4 2_555 . 2_555 91.3(3) ?
I1 Pb2 I4 6_555 . . 88.7(3) ?
I1 Pb2 I4 6_555 . 2_555 88.9(3) ?
I4 Pb2 I4 . . 2_555 176.6(4) ?
Pb2 I1 Pb2 . . 5_545 177.2(3) ?
Pb1 I2 Pb1 . . 5_545 176.6(3) ?
Pb1 I2 N1 . . . 91.1(12) ?
Pb1 I2 N1 5_545 . . 88.3(12) ?
Pb1 I3 Pb1 . . 5_555 176.8(3) ?
Pb1 I3 N2 . . . 93.9(9) ?
Pb1 I3 N2 5_555 . . 89.2(9) ?
Pb1 I4 Pb2 . . . 176.7(5) ?
Pb1 I4 N2 . . . 87.0(10) ?
Pb1 I4 N2 . . 5_445 85.0(10) ?
Pb2 I4 N2 . . . 96.2(10) ?
Pb2 I4 N2 . . 5_445 94.3(10) ?
N2 I4 N2 . . 5_445 119.8(12) ?
I2 N1 C1a . . . 130(5) ?
I2 N1 H1n1 . . . 108.49 ?
I2 N1 H2n1 . . . 86.27 ?
I2 N1 H3n1 . . . 25.9 ?
C1a N1 H1n1 . . . 109.47 ?
C1a N1 H2n1 . . . 109.47 ?
C1a N1 H3n1 . . . 109.47 ?
H1n1 N1 H2n1 . . . 109.47 ?
H1n1 N1 H3n1 . . . 109.47 ?
H2n1 N1 H3n1 . . . 109.47 ?
N1 C1a C1b . . . 109(5) ?
N1 C1a H1c1a . . . 109.47 ?
N1 C1a H2c1a . . . 109.47 ?
C1b C1a H1c1a . . . 109.47 ?
C1b C1a H2c1a . . . 109.47 ?
H1c1a C1a H2c1a . . . 109.47 ?
I3 N2 I4 . . . 76.8(12) ?
I3 N2 I4 . . 5_555 80.8(11) ?
I3 N2 C2 . . . 144(4) ?
I3 N2 H1n2 . . . 64.26 ?
I3 N2 H2n2 . . . 49.61 ?
I3 N2 H3n2 . . . 106.08 ?
I4 N2 I4 . . 5_555 119.8(15) ?
I4 N2 C2 . . . 113(4) ?
I4 N2 H1n2 . . . 24.31 ?
I4 N2 H2n2 . . . 126.3 ?
I4 N2 H3n2 . . . 86.25 ?
I4 N2 C2 5_555 . . 118(4) ?
I4 N2 H1n2 5_555 . . 131.8 ?
I4 N2 H2n2 5_555 . . 61.79 ?
I4 N2 H3n2 5_555 . . 48.27 ?
C2 N2 H1n2 . . . 109.47 ?
C2 N2 H2n2 . . . 109.47 ?
C2 N2 H3n2 . . . 109.47 ?
H1n2 N2 H2n2 . . . 109.47 ?
H1n2 N2 H3n2 . . . 109.47 ?
H2n2 N2 H3n2 . . . 109.47 ?
N2 C2 H1c2 . . . 109.47 ?
N2 C2 H2c2 . . . 109.47 ?
N2 C2 H3c2 . . . 109.47 ?
H1c2 C2 H2c2 . . . 109.47 ?
H1c2 C2 H3c2 . . . 109.47 ?
H2c2 C2 H3c2 . . . 109.47 ?
C1a C1b C1c . . . 109(6) ?
C1a C1b C1d . . . 109(6) ?
C1a C1b H1c1b . . . 109.47 ?
C1c C1b C1d . . . 109(6) ?
C1c C1b H1c1b . . . 109.47 ?
C1d C1b H1c1b . . . 109.47 ?
C1b C1c H1c1c . . . 109.47 ?
C1b C1c H2c1c . . . 109.47 ?
C1b C1c H3c1c . . . 109.47 ?
H1c1c C1c H2c1c . . . 109.47 ?
H1c1c C1c H3c1c . . . 109.47 ?
H2c1c C1c H3c1c . . . 109.47 ?
C1b C1d H1c1d . . . 109.47 ?
C1b C1d H2c1d . . . 109.47 ?
C1b C1d H3c1d . . . 109.47 ?
H1c1d C1d H2c1d . . . 109.47 ?
H1c1d C1d H3c1d . . . 109.47 ?
H2c1d C1d H3c1d . . . 109.47 ?

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
C1d H2c1d N1 . . . 0.96 2.01 2.56(10) 114.65 ?
N1 H2n1 C1d . . . 0.87 2.02 2.56(10) 119.22 ?


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Hydriodic Acid'
####################################################################### 
# 
# 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_I_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 2018085'
loop_
_audit_author_name
_audit_author_address
'Justin Hoffman'
;Northwestern University
United States of America
;
_audit_update_record             
;
2020-07-21 deposited with the CCDC.	2020-10-06 downloaded from the CCDC.
;
#=======================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic        
; ?
;
_chemical_name_common            ?
_chemical_formula_moiety         '2(C4 H12 N 1+), (C H6 N 1+), Pb2 I7 3-'
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_iupac          ?
_chemical_formula_sum            'C9 H30 I7 N3 Pb2'
_chemical_formula_weight         1483.1
_chemical_melting_point          ?
_chemical_compound_source        ?
_chemical_absolute_configuration .

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

# 6. CRYSTAL DATA

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_Int_Tables_number      15

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

_cell_length_a                   38.9330(15)
_cell_length_b                   8.9419(2)
_cell_length_c                   8.8520(3)
_cell_angle_alpha                90
_cell_angle_beta                 90.112(3)
_cell_angle_gamma                90
_cell_volume                     3081.69(17)

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
? ? ? ? ? ? ? ? ? ? ?

_cell_formula_units_Z            4

_cell_measurement_reflns_used    5644
_cell_measurement_theta_min      2.74
_cell_measurement_theta_max      27.41
_cell_measurement_temperature    285(14)
_cell_special_details            
; ?
;

_exptl_crystal_density_diffrn    3.1966
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             2572

_exptl_absorpt_coefficient_mu    17.924
_exptl_crystal_description       plate
_exptl_crystal_size_max          0.076
_exptl_crystal_size_mid          0.029
_exptl_crystal_size_min          0.013
_exptl_crystal_size_rad          ?
_exptl_crystal_colour            red
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.25a (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.366
_exptl_absorpt_correction_T_max  0.808
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      285
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_power             ?
_diffrn_source_voltage           ?
_diffrn_source_current           ?
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       ?
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support ?

_diffrn_reflns_number            13230
_diffrn_reflns_theta_min         2.77
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_full        27.32
_diffrn_measured_fraction_theta_max 0.98
_diffrn_measured_fraction_theta_full 0.98
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_av_unetI/netI     0.0213
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       9
_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          
; The structure was refined based on the following considerations.
 The perovskite lattice was refined anisotropically without
 any constraints on the Pb and I atoms. The highly anisotropic shape of
 the thermal ellipsoids of coordinated iodide ions appears due to a high
 thermal motion relative to the Pb-I bond vector. It is typical for the
 halide perovskites structures at room temperature and therefore no 
 special treatment was used. All organic atoms were refined isotropically.
 Restraints were applied to the C-C and C-N bond lengths. Each cation was
 treated as having equivalent thermal parameters. Significant disorder 
 exists in the interlayer cations,  causing the atoms to move and destabilize the refinement. 
 The bond length restraints cannot account for the motion of the interlayer cations. 
 Therefore the cations were modeled manually based on reasonable
 bond length and bond angle parameters. 
;

_reflns_number_total             2768
_reflns_number_gt                2377
_reflns_threshold_expression     I>3σ(I)

_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_gt           0.0667
_refine_ls_wR_factor_gt          0.2027
_refine_ls_R_factor_all          0.0730
_refine_ls_wR_factor_ref         0.2033
_refine_ls_goodness_of_fit_ref   5.41
_refine_ls_goodness_of_fit_gt    5.83
_refine_ls_restrained_S_gt       ?
_refine_ls_restrained_S_all      ?
_refine_ls_number_reflns         2768
_refine_ls_number_parameters     62
_refine_ls_number_restraints     9
_refine_ls_number_constraints    68
_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          0.0474
_refine_ls_shift/su_mean         0.0042
_refine_diff_density_max         3.12
_refine_diff_density_min         -2.58
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_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 0.0033 0.0016 '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 -0.4742 1.8119 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
N 0.0061 0.0033 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
Pb -3.3944 10.1111 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'

_computing_data_collection       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_structure_solution    ?
_computing_structure_refinement  ?
_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
N2 . C2a . 1.5 0.001
C2a . C2b . 1.5 0.001
C2b . C2c . 1.5 0.001
C2b . C2d . 1.5 0.001
C1a 2_755 N1a . 1.5 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
N2 . C2a . C2b . 109.47 0.01
C2a . C2b . C2c . 109.47 0.01
C2a . C2b . C2d . 109.47 0.01
C2c . C2b . C2d . 109.47 0.01

loop_
_restr_torsion_atom_site_label_1
_restr_torsion_site_symmetry_1
_restr_torsion_atom_site_label_2
_restr_torsion_site_symmetry_2
_restr_torsion_atom_site_label_3
_restr_torsion_site_symmetry_3
_restr_torsion_atom_site_label_4
_restr_torsion_site_symmetry_4
_restr_torsion_angle_target
_restr_torsion_weight_param
? ? ? ? ? ? ? ? ? ?

loop_
_restr_equal_distance_atom_site_label_1
_restr_equal_distance_site_symmetry_1
_restr_equal_distance_atom_site_label_2
_restr_equal_distance_site_symmetry_2
_restr_equal_distance_class_class_id
_restr_equal_distance_class_target_weight_param
? ? ? ? ? ?

loop_
_restr_equal_angle_atom_site_label_1
_restr_equal_angle_site_symmetry_1
_restr_equal_angle_atom_site_label_2
_restr_equal_angle_site_symmetry_2
_restr_equal_angle_atom_site_label_3
_restr_equal_angle_site_symmetry_3
_restr_equal_angle_class_class_id
_restr_equal_angle_class_target_weight_param
? ? ? ? ? ? ? ?

loop_
_restr_equal_torsion_atom_site_label_1
_restr_equal_torsion_site_symmetry_1
_restr_equal_torsion_atom_site_label_2
_restr_equal_torsion_site_symmetry_2
_restr_equal_torsion_atom_site_label_3
_restr_equal_torsion_site_symmetry_3
_restr_equal_torsion_atom_site_label_4
_restr_equal_torsion_site_symmetry_4
_restr_equal_torsion_class_class_id
_restr_equal_torsion_class_target_weight_param
? ? ? ? ? ? ? ? ? ?


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

# 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 0.416446(17) 0.24863(7) 0.25033(8) Uani 0.0412(3) 8 1 d . . .
I1 I 0.5 0.2418(3) 0.25 Uani 0.0708(9) 4 1 d . . .
I2 I 0.07917(4) 0.04346(16) 0.04371(17) Uani 0.0672(5) 8 1 d . . .
I3 I 0.91598(5) 0.45528(17) 0.04494(18) Uani 0.0735(6) 8 1 d . . .
I4 I 0.66341(4) 0.2853(2) 0.2388(2) Uani 0.0806(7) 8 1 d . . .
C2a C 0.6645(6) 0.801(3) 0.223(4) Uiso 0.163(7) 8 1 d . . .
N2 N 0.6480(7) 0.687(3) 0.325(4) Uiso 0.163(7) 8 1 d . . .
C2c C 0.7193(7) 0.884(4) 0.117(4) Uiso 0.163(7) 8 1 d . . .
C2b C 0.7016(6) 0.761(2) 0.201(3) Uiso 0.163(7) 8 1 d . . .
C1a C 1.0074(13) 0.289(4) 0.172(2) Uiso 0.29(2) 8 1 d . . .
C2d C 0.7186(7) 0.739(4) 0.351(3) Uiso 0.163(7) 8 1 d . . .
H1c2a H 0.662965 0.897912 0.268629 Uiso 0.1951 8 1 d . . .
H2c2a H 0.652969 0.801383 0.127393 Uiso 0.1951 8 1 d . . .
H1c2c H 0.704445 0.970099 0.111971 Uiso 0.1951 8 1 d . . .
H2c2c H 0.740129 0.910717 0.16826 Uiso 0.1951 8 1 d . . .
H3c2c H 0.724551 0.851622 0.01612 Uiso 0.1951 8 1 d . . .
H1c2b H 0.70315 0.669861 0.143381 Uiso 0.1951 8 1 d . . .
H1c2d H 0.734935 0.659382 0.344901 Uiso 0.1951 8 1 d . . .
H2c2d H 0.730094 0.829884 0.380157 Uiso 0.1951 8 1 d . . .
H3c2d H 0.701484 0.715091 0.425556 Uiso 0.1951 8 1 d . . .
H1n2 H 0.63602 0.733093 0.393562 Uiso 0.1951 8 1 d . . .
H2n2 H 0.634609 0.629833 0.271731 Uiso 0.1951 8 1 d . . .
H3n2 H 0.663837 0.633482 0.368 Uiso 0.1951 8 1 d . . .
N1a N 1.0074(13) 0.289(4) 0.172(2) Uiso 0.29(2) 8 0.5 d . . .
H1n1 H 1.010495 0.19771 0.14205 Uiso 0.344 8 0.5 d . . .
H2n1 H 0.993249 0.33422 0.110445 Uiso 0.344 8 0.5 d . . .
H3n1 H 1.026953 0.336365 0.17221 Uiso 0.344 8 0.5 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 . . 3.2536(7) ?
Pb1 I2 . 6_555 3.2097(16) ?
Pb1 I2 . 7_555 3.2034(16) ?
Pb1 I3 . 5_445 3.1916(16) ?
Pb1 I3 . 8_455 3.1822(17) ?
Pb1 I4 . 2_655 3.1278(17) ?
I1 N1a . 7_655 3.75(2) ?
I1 N1a . 8_455 3.75(2) ?
I2 N1a . 1_455 3.73(4) ?
I3 N2 . 6_645 3.65(3) ?
I4 N2 . . 3.72(3) ?
I4 N2 . 4_564 3.72(3) ?
C2a N2 . . 1.50(4) ?
C2a C2b . . 1.50(3) ?
C2a H1c2a . . 0.96 ?
C2a H2c2a . . 0.96 ?
N2 H1n2 . . 0.87 ?
N2 H2n2 . . 0.87 ?
N2 H3n2 . . 0.87 ?
C2c C2b . . 1.50(4) ?
C2c H1c2c . . 0.96 ?
C2c H2c2c . . 0.96 ?
C2c H3c2c . . 0.96 ?
C2b C2d . . 1.50(4) ?
C2b H1c2b . . 0.96 ?
C1a C1a . 2_755 1.50(4) ?
C1a N1a . . 0 ?
C1a N1a . 2_755 1.50(4) ?
C1a H1n1 . . 0.87 ?
C1a H2n1 . . 0.87 ?
C1a H3n1 . . 0.87 ?
C2d H1c2d . . 0.96 ?
C2d H2c2d . . 0.96 ?
C2d H3c2d . . 0.96 ?
N1a N1a . 2_755 1.50(4) ?
N1a H1n1 . . 0.87 ?
N1a H2n1 . . 0.87 ?
N1a H3n1 . . 0.87 ?

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 . . 6_555 87.93(5) ?
I1 Pb1 I2 . . 7_555 87.44(4) ?
I1 Pb1 I3 . . 5_445 89.35(5) ?
I1 Pb1 I3 . . 8_455 89.85(4) ?
I1 Pb1 I4 . . 2_655 174.76(6) ?
I2 Pb1 I2 6_555 . 7_555 88.97(4) ?
I2 Pb1 I3 6_555 . 5_445 177.28(5) ?
I2 Pb1 I3 6_555 . 8_455 90.32(4) ?
I2 Pb1 I4 6_555 . 2_655 87.03(5) ?
I2 Pb1 I3 7_555 . 5_445 90.82(4) ?
I2 Pb1 I3 7_555 . 8_455 177.21(5) ?
I2 Pb1 I4 7_555 . 2_655 91.07(5) ?
I3 Pb1 I3 5_445 . 8_455 89.76(4) ?
I3 Pb1 I4 5_445 . 2_655 95.69(5) ?
I3 Pb1 I4 8_455 . 2_655 91.59(5) ?
Pb1 I1 Pb1 . . 2_655 177.85(9) ?
Pb1 I1 N1a . . 7_655 85.9(8) ?
Pb1 I1 N1a . . 8_455 94.3(8) ?
Pb1 I1 N1a 2_655 . 7_655 94.3(8) ?
Pb1 I1 N1a 2_655 . 8_455 85.9(8) ?
N1a I1 N1a 7_655 . 8_455 171.5(8) ?
Pb1 I2 Pb1 6_545 . 7_555 159.28(6) ?
Pb1 I2 N1a 6_545 . 1_455 110.5(5) ?
Pb1 I2 N1a 7_555 . 1_455 86.9(4) ?
Pb1 I3 Pb1 5_555 . 8_554 159.68(6) ?
Pb1 I3 N2 5_555 . 6_645 111.3(5) ?
Pb1 I3 N2 8_554 . 6_645 83.6(5) ?
Pb1 I4 N2 2_655 . . 86.3(4) ?
Pb1 I4 N2 2_655 . 4_564 83.0(4) ?
N2 I4 N2 . . 4_564 96.5(7) ?
N2 C2a C2b . . . 109(2) ?
N2 C2a H1c2a . . . 109.47 ?
N2 C2a H2c2a . . . 109.47 ?
C2b C2a H1c2a . . . 109.47 ?
C2b C2a H2c2a . . . 109.47 ?
H1c2a C2a H2c2a . . . 109.47 ?
I3 N2 I4 6_655 . . 144.1(8) ?
I3 N2 I4 6_655 . 4_565 75.8(6) ?
I3 N2 C2a 6_655 . . 92.3(15) ?
I3 N2 H1n2 6_655 . . 26.06 ?
I3 N2 H2n2 6_655 . . 98.61 ?
I3 N2 H3n2 6_655 . . 135.13 ?
I4 N2 I4 . . 4_565 103.8(7) ?
I4 N2 C2a . . . 117.4(18) ?
I4 N2 H1n2 . . . 133.12 ?
I4 N2 H2n2 . . . 54.22 ?
I4 N2 H3n2 . . . 56.01 ?
I4 N2 C2a 4_565 . . 118.5(19) ?
I4 N2 H1n2 4_565 . . 50.63 ?
I4 N2 H2n2 4_565 . . 131.76 ?
I4 N2 H3n2 4_565 . . 59.39 ?
C2a N2 H1n2 . . . 109.47 ?
C2a N2 H2n2 . . . 109.47 ?
C2a N2 H3n2 . . . 109.47 ?
H1n2 N2 H2n2 . . . 109.47 ?
H1n2 N2 H3n2 . . . 109.47 ?
H2n2 N2 H3n2 . . . 109.47 ?
C2b C2c H1c2c . . . 109.47 ?
C2b C2c H2c2c . . . 109.47 ?
C2b C2c H3c2c . . . 109.47 ?
H1c2c C2c H2c2c . . . 109.47 ?
H1c2c C2c H3c2c . . . 109.47 ?
H2c2c C2c H3c2c . . . 109.47 ?
C2a C2b C2c . . . 109(2) ?
C2a C2b C2d . . . 109(2) ?
C2a C2b H1c2b . . . 109.47 ?
C2c C2b C2d . . . 109(2) ?
C2c C2b H1c2b . . . 109.47 ?
C2d C2b H1c2b . . . 109.47 ?
C1a C1a N1a 2_755 . . 0 ?
C1a C1a N1a 2_755 . 2_755 0.0(5) ?
C1a C1a H1n1 2_755 . . 109.47 ?
C1a C1a H2n1 2_755 . . 109.47 ?
C1a C1a H3n1 2_755 . . 109.47 ?
N1a C1a N1a . . 2_755 0 ?
N1a C1a H1n1 . . . 0 ?
N1a C1a H2n1 . . . 0 ?
N1a C1a H3n1 . . . 0 ?
N1a C1a H1n1 2_755 . . 109.47 ?
N1a C1a H2n1 2_755 . . 109.47 ?
N1a C1a H3n1 2_755 . . 109.47 ?
H1n1 C1a H2n1 . . . 109.47 ?
H1n1 C1a H3n1 . . . 109.47 ?
H2n1 C1a H3n1 . . . 109.47 ?
C2b C2d H1c2d . . . 109.47 ?
C2b C2d H2c2d . . . 109.47 ?
C2b C2d H3c2d . . . 109.47 ?
H1c2d C2d H2c2d . . . 109.47 ?
H1c2d C2d H3c2d . . . 109.47 ?
H2c2d C2d H3c2d . . . 109.47 ?
I1 N1a I2 7_655 . 1_655 73.1(6) ?
I1 N1a C1a 7_655 . . 0 ?
I1 N1a C1a 7_655 . 2_755 153(3) ?
I1 N1a N1a 7_655 . 2_755 153(3) ?
I1 N1a H1n1 7_655 . . 68.85 ?
I1 N1a H2n1 7_655 . . 50.68 ?
I1 N1a H3n1 7_655 . . 96.04 ?
I2 N1a C1a 1_655 . . 0 ?
I2 N1a C1a 1_655 . 2_755 125(2) ?
I2 N1a N1a 1_655 . 2_755 125(2) ?
I2 N1a H1n1 1_655 . . 41.24 ?
I2 N1a H2n1 1_655 . . 123.66 ?
I2 N1a H3n1 1_655 . . 68.24 ?
C1a N1a C1a . . 2_755 0 ?
C1a N1a N1a . . 2_755 0 ?
C1a N1a H1n1 . . . 0 ?
C1a N1a H2n1 . . . 0 ?
C1a N1a H3n1 . . . 0 ?
C1a N1a N1a 2_755 . 2_755 0.0(5) ?
C1a N1a H1n1 2_755 . . 109.47 ?
C1a N1a H2n1 2_755 . . 109.47 ?
C1a N1a H3n1 2_755 . . 109.47 ?
N1a N1a H1n1 2_755 . . 109.47 ?
N1a N1a H2n1 2_755 . . 109.47 ?
N1a N1a H3n1 2_755 . . 109.47 ?
H1n1 N1a H2n1 . . . 109.47 ?
H1n1 N1a H3n1 . . . 109.47 ?
H2n1 N1a H3n1 . . . 109.47 ?
C1a H1n1 N1a . . . 0 ?
C1a H2n1 N1a . . . 0 ?
C1a H3n1 N1a . . . 0 ?

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
C2d H3c2d N2 . . . 0.96 2.28 2.79(4) 112.97 ?
N2 H3n2 C2d . . . 0.87 2.34 2.79(4) 113.13 ?


####################################################################### 
# 
# 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_I_CCDC4
_database_code_depnum_ccdc_archive 'CCDC 2018087'
loop_
_audit_author_name
_audit_author_address
'Justin Hoffman'
;Northwestern University
United States of America
;
_audit_update_record             
;
2020-07-21 deposited with the CCDC.	2020-10-06 downloaded from the CCDC.
;
#=======================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic        
; ?
;
_chemical_name_common            ?
_chemical_formula_moiety         '2(C5 H14 N 1+), 3(C H6 N 1+), Pb4 I13 5-'
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_iupac          ?
_chemical_formula_sum            'C13 H46 I13 N5 Pb4'
_chemical_formula_weight         2751.1
_chemical_melting_point          ?
_chemical_compound_source        ?
_chemical_absolute_configuration .

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

# 6. CRYSTAL DATA

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_Int_Tables_number      12

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

_cell_length_a                   8.9275(10)
_cell_length_b                   68.140(10)
_cell_length_c                   8.9142(10)
_cell_angle_alpha                90
_cell_angle_beta                 90.551(9)
_cell_angle_gamma                90
_cell_volume                     5422.4(12)

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
? ? ? ? ? ? ? ? ? ? ?

_cell_formula_units_Z            4

_cell_measurement_reflns_used    1817
_cell_measurement_theta_min      2.39
_cell_measurement_theta_max      27.71
_cell_measurement_temperature    293
_cell_special_details            
; ?
;

_exptl_crystal_density_diffrn    3.3699
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             4704

_exptl_absorpt_coefficient_mu    19.797
_exptl_crystal_description       plate
_exptl_crystal_size_max          0.1830
_exptl_crystal_size_mid          0.1093
_exptl_crystal_size_min          0.0684
_exptl_crystal_size_rad          ?
_exptl_crystal_colour            black
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   ?
_exptl_absorpt_correction_T_min  0.0483
_exptl_absorpt_correction_T_max  0.1279
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
15 0 -8 0.1171
2 1 30 0.0684
1 0 10 0.0927
15 -7 -5 0.1643
2 0 -15 0.0814
1 15 -3 0.1830
-1 -1 -15 0.0962
-1 0 -10 0.0791
-30 13 6 0.1173
-4 1 30 0.1217
-3 -2 30 0.0959
1 -30 12 0.1692
-1 2 -30 0.1093

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

# 7. EXPERIMENTAL DATA

_exptl_special_details           ?

_diffrn_ambient_temperature      293
_diffrn_source                   ?
_diffrn_source_power             ?
_diffrn_source_voltage           ?
_diffrn_source_current           ?
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'IPDS Stoe'
_diffrn_detector                 ?
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_method       '??integration method??'
_diffrn_measurement_specimen_support ?

_diffrn_reflns_number            28026
_diffrn_reflns_theta_min         1.79
_diffrn_reflns_theta_max         29.3
_diffrn_reflns_theta_full        29.27
_diffrn_measured_fraction_theta_max 0.97
_diffrn_measured_fraction_theta_full 0.97
_diffrn_reflns_av_R_equivalents  0.3061
_diffrn_reflns_av_unetI/netI     0.47
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -88
_diffrn_reflns_limit_k_max       93
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_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          
; The structure was refined based on the following considerations.
 The perovskite lattice was refined anisotropically without
 any constraints on the Pb and I atoms. The highly anisotropic shape of
 the thermal ellipsoids of coordinated iodide ions appears due to a high
 thermal motion relative to the Pb-I bond vector. It is typical for the
 halide perovskites structures at room temperature and therefore no 
 special treatment was used. All organic atoms were refined isotropically.
 Restraints were applied to the C-C and C-N bond lengths. Each cation was
 treated as having equivalent thermal parameters. Significant disorder 
 exists in the interlayer cations,  causing the atoms to move and destabilize the refinement. 
 The bond length restraints cannot account for the motion of the interlayer cations. 
 Therefore the cations were modeled manually based on reasonable
 bond length and bond angle parameters. Some of these cations are shown
 unreasonably close to one another due to this disorder. Furthermore,
 as the crystal often co-precipitates with other n values,
 this structure had other phases grown on its surface, leading to a large amount
 of the data being discluded, leading to a low ratio of observed/unique reflections.
;

_reflns_number_total             4785
_reflns_number_gt                399
_reflns_threshold_expression     I>3σ(I)

_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_gt           0.0951
_refine_ls_wR_factor_gt          0.1971
_refine_ls_R_factor_all          0.3343
_refine_ls_wR_factor_ref         0.2309
_refine_ls_goodness_of_fit_ref   0.80
_refine_ls_goodness_of_fit_gt    2.71
_refine_ls_restrained_S_gt       ?
_refine_ls_restrained_S_all      ?
_refine_ls_number_reflns         4785
_refine_ls_number_parameters     114
_refine_ls_number_restraints     12
_refine_ls_number_constraints    111
_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          0.0499
_refine_ls_shift/su_mean         0.0038
_refine_diff_density_max         1.95
_refine_diff_density_min         -2.56
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_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 0.0033 0.0016 '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 -0.4742 1.8119 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
N 0.0061 0.0033 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
Pb -3.3944 10.1111 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  ?
_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
N2 . C2a . 1.5 0.001
N3 . C3a . 1.5 0.001
N4 . C4a . 1.5 0.001
C4a . C4b . 1.5 0.001
C4b . C4c . 1.5 0.001
C4c . C4d . 1.5 0.001
C4c . C4e . 1.5 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 . C4a . C4b . 109.47 0.01
C4a . C4b . C4c . 109.47 0.01
C4b . C4c . C4d . 109.47 0.01
C4b . C4c . C4e . 109.47 0.01
C4d . C4c . C4e . 109.47 0.01

loop_
_restr_torsion_atom_site_label_1
_restr_torsion_site_symmetry_1
_restr_torsion_atom_site_label_2
_restr_torsion_site_symmetry_2
_restr_torsion_atom_site_label_3
_restr_torsion_site_symmetry_3
_restr_torsion_atom_site_label_4
_restr_torsion_site_symmetry_4
_restr_torsion_angle_target
_restr_torsion_weight_param
? ? ? ? ? ? ? ? ? ?

loop_
_restr_equal_distance_atom_site_label_1
_restr_equal_distance_site_symmetry_1
_restr_equal_distance_atom_site_label_2
_restr_equal_distance_site_symmetry_2
_restr_equal_distance_class_class_id
_restr_equal_distance_class_target_weight_param
? ? ? ? ? ?

loop_
_restr_equal_angle_atom_site_label_1
_restr_equal_angle_site_symmetry_1
_restr_equal_angle_atom_site_label_2
_restr_equal_angle_site_symmetry_2
_restr_equal_angle_atom_site_label_3
_restr_equal_angle_site_symmetry_3
_restr_equal_angle_class_class_id
_restr_equal_angle_class_target_weight_param
? ? ? ? ? ? ? ?

loop_
_restr_equal_torsion_atom_site_label_1
_restr_equal_torsion_site_symmetry_1
_restr_equal_torsion_atom_site_label_2
_restr_equal_torsion_site_symmetry_2
_restr_equal_torsion_atom_site_label_3
_restr_equal_torsion_site_symmetry_3
_restr_equal_torsion_atom_site_label_4
_restr_equal_torsion_site_symmetry_4
_restr_equal_torsion_class_class_id
_restr_equal_torsion_class_target_weight_param
? ? ? ? ? ? ? ? ? ?


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

# 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 0.2487(7) 0.04679(7) 0.2493(7) Uani 0.0723(12) 8 1 d . . .
Pb2 Pb 0.2511(6) 0.14087(5) 0.2497(5) Uani 0.0735(14) 8 1 d . . .
I1 I 0.2872(12) 0.09228(12) 0.2748(11) Uani 0.125(4) 8 1 d . . .
I2 I 0.235(2) 0 0.2123(10) Uani 0.149(7) 4 1 d . . .
I3 I 0.5 0.1397(3) 0 Uani 0.148(9) 4 1 d . . .
I4 I 0.5 0.1442(3) 0.5 Uani 0.147(8) 4 1 d . . .
I5 I 0 0.1341(2) 0 Uani 0.136(7) 4 1 d . . .
I6 I 0 0.1394(3) 0.5 Uani 0.131(7) 4 1 d . . .
I7 I 0 0.0519(3) 0 Uani 0.166(9) 4 1 d . . .
I8 I 0.2078(16) 0.18489(12) 0.2184(15) Uani 0.175(7) 8 1 d . . .
I9 I 0 0.0470(3) 0.5 Uani 0.134(8) 4 1 d . . .
I10 I 0.5 0.0466(3) 0 Uani 0.200(11) 4 1 d . . .
I11 I 0.5 0.0418(3) 0.5 Uani 0.158(9) 4 1 d . . .
N2 N 0.398(6) 0 0.571(7) Uiso 0.058(17) 4 1 d . . .
N3 N -0.043(8) 0.0929(12) 0.177(7) Uiso 0.15(2) 8 1 d . . .
N4 N 0.214(13) 0.1699(11) -0.318(11) Uiso 0.22(3) 8 1 d . . .
C3a C -0.180(8) 0.0917(13) 0.272(9) Uiso 0.15(2) 8 1 d . . .
C2a C 0.288(7) 0 0.697(7) Uiso 0.058(17) 4 1 d . . .
C4a C 0.227(15) 0.1832(11) -0.185(10) Uiso 0.22(3) 8 1 d . . .
C4b C 0.335(8) 0.1994(10) -0.217(12) Uiso 0.22(3) 8 1 d . . .
C4c C 0.264(9) 0.2188(10) -0.183(7) Uiso 0.22(3) 8 1 d . . .
C4d C 0.367(13) 0.2306(11) -0.085(8) Uiso 0.22(3) 8 1 d . . .
C4e C 0.235(15) 0.2297(13) -0.327(4) Uiso 0.22(3) 8 1 d . . .
H1c3a H -0.209322 0.078232 0.283565 Uiso 0.1852 8 1 d . . .
H2c3a H -0.159135 0.097284 0.368861 Uiso 0.1852 8 1 d . . .
H3c3a H -0.260593 0.098877 0.224859 Uiso 0.1852 8 1 d . . .
H1c2a H 0.266126 -0.013278 0.725663 Uiso 0.0698 8 0.5 d . . .
H2c2a H 0.329014 0.006966 0.781195 Uiso 0.0698 8 0.5 d . . .
H3c2a H 0.196721 0.006312 0.664376 Uiso 0.0698 8 0.5 d . . .
H1c4a H 0.261433 0.175847 -0.099465 Uiso 0.2636 8 1 d . . .
H2c4a H 0.130011 0.188706 -0.163537 Uiso 0.2636 8 1 d . . .
H1c4b H 0.423339 0.1978 -0.156386 Uiso 0.2636 8 1 d . . .
H2c4b H 0.361843 0.199 -0.321451 Uiso 0.2636 8 1 d . . .
H1c4c H 0.170839 0.216692 -0.132326 Uiso 0.2636 8 1 d . . .
H1c4d H 0.467545 0.229509 -0.120608 Uiso 0.2636 8 1 d . . .
H2c4d H 0.336745 0.244164 -0.086931 Uiso 0.2636 8 1 d . . .
H3c4d H 0.362289 0.225816 0.016292 Uiso 0.2636 8 1 d . . .
H1c4e H 0.319847 0.228529 -0.390767 Uiso 0.2636 8 1 d . . .
H2c4e H 0.148002 0.2243 -0.376098 Uiso 0.2636 8 1 d . . .
H3c4e H 0.217124 0.24333 -0.304894 Uiso 0.2636 8 1 d . . .
H1n2 H 0.448389 -0.010925 0.572522 Uiso 0.0698 8 0.5 d . . .
H2n2 H 0.35035 0.001085 0.48595 Uiso 0.0698 8 0.5 d . . .
H3n2 H 0.459204 0.00984 0.582072 Uiso 0.0698 8 0.5 d . . .
H1n3 H 0.008193 0.082111 0.186002 Uiso 0.1852 8 1 d . . .
H2n3 H -0.069814 0.094434 0.083152 Uiso 0.1852 8 1 d . . .
H3n3 H 0.011344 0.102805 0.205178 Uiso 0.1852 8 1 d . . .
H1n4 H 0.245958 0.158238 -0.294005 Uiso 0.2636 8 1 d . . .
H2n4 H 0.121156 0.169209 -0.34762 Uiso 0.2636 8 1 d . . .
H3n4 H 0.268481 0.17452 -0.390748 Uiso 0.2636 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 . . 3.127(10) ?
Pb1 I2 . . 3.208(5) ?
Pb1 I7 . . 3.146(6) ?
Pb1 I9 . . 3.166(6) ?
Pb1 I10 . . 3.172(6) ?
Pb1 I11 . . 3.170(6) ?
Pb2 I1 . . 3.334(9) ?
Pb2 I3 . . 3.161(5) ?
Pb2 I4 . . 3.142(5) ?
Pb2 I5 . . 3.177(6) ?
Pb2 I6 . . 3.180(5) ?
Pb2 I8 . . 3.037(9) ?
I1 N3 . . 3.07(7) ?
I2 N2 . . 3.50(6) ?
I2 N2 . 2_656 3.79(6) ?
I4 N4 . 1_556 3.50(10) ?
I4 N4 . 2_655 3.50(10) ?
I5 N3 . . 3.24(8) ?
I5 N3 . 2_555 3.24(8) ?
I6 N4 . 1_556 3.25(10) ?
I6 N4 . 2_555 3.25(10) ?
I7 N3 . . 3.23(8) ?
I7 N3 . 2_555 3.23(8) ?
I11 N2 . . 3.06(3) ?
I11 N2 . 2_656 3.06(3) ?

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 . . . 175.6(4) ?
I1 Pb1 I7 . . . 91.0(4) ?
I1 Pb1 I9 . . . 91.3(4) ?
I1 Pb1 I10 . . . 88.7(4) ?
I1 Pb1 I11 . . . 88.8(4) ?
I2 Pb1 I7 . . . 90.7(5) ?
I2 Pb1 I9 . . . 92.8(4) ?
I2 Pb1 I10 . . . 87.2(5) ?
I2 Pb1 I11 . . . 89.5(4) ?
I7 Pb1 I9 . . . 90.18(16) ?
I7 Pb1 I10 . . . 90.27(16) ?
I7 Pb1 I11 . . . 179.8(4) ?
I9 Pb1 I10 . . . 179.5(2) ?
I9 Pb1 I11 . . . 89.94(16) ?
I10 Pb1 I11 . . . 89.61(15) ?
I1 Pb2 I3 . . . 87.4(4) ?
I1 Pb2 I4 . . . 87.5(4) ?
I1 Pb2 I5 . . . 88.3(3) ?
I1 Pb2 I6 . . . 89.5(4) ?
I1 Pb2 I8 . . . 177.7(4) ?
I3 Pb2 I4 . . . 90.27(15) ?
I3 Pb2 I5 . . . 89.96(13) ?
I3 Pb2 I6 . . . 176.8(5) ?
I3 Pb2 I8 . . . 92.8(5) ?
I4 Pb2 I5 . . . 175.7(5) ?
I4 Pb2 I6 . . . 90.13(12) ?
I4 Pb2 I8 . . . 94.8(4) ?
I5 Pb2 I6 . . . 89.40(15) ?
I5 Pb2 I8 . . . 89.5(4) ?
I6 Pb2 I8 . . . 90.3(4) ?
Pb1 I1 Pb2 . . . 165.7(4) ?
Pb1 I1 N3 . . . 83.6(16) ?
Pb2 I1 N3 . . . 82.8(16) ?
Pb1 I2 Pb1 . . 4_555 167.4(4) ?
Pb1 I2 N2 . . . 83.7(2) ?
Pb1 I2 N2 . . 2_656 85.1(3) ?
Pb1 I2 N2 4_555 . . 83.7(2) ?
Pb1 I2 N2 4_555 . 2_656 85.1(3) ?
N2 I2 N2 . . 2_656 35.3(13) ?
Pb2 I3 Pb2 . . 2_655 177.2(7) ?
Pb2 I4 Pb2 . . 2_656 171.8(7) ?
Pb2 I4 N4 . . 1_556 81.4(17) ?
Pb2 I4 N4 . . 2_655 102.7(17) ?
Pb2 I4 N4 2_656 . 1_556 102.7(17) ?
Pb2 I4 N4 2_656 . 2_655 81.4(17) ?
N4 I4 N4 1_556 . 2_655 120(2) ?
Pb2 I5 Pb2 . . 2_555 163.3(6) ?
Pb2 I5 N3 . . . 82.7(13) ?
Pb2 I5 N3 . . 2_555 112.3(13) ?
Pb2 I5 N3 2_555 . . 112.3(13) ?
Pb2 I5 N3 2_555 . 2_555 82.7(13) ?
N3 I5 N3 . . 2_555 60.1(18) ?
Pb2 I6 Pb2 . . 2_556 176.5(6) ?
Pb2 I6 N4 . . 1_556 85.1(19) ?
Pb2 I6 N4 . . 2_555 92.6(19) ?
Pb2 I6 N4 2_556 . 1_556 92.6(19) ?
Pb2 I6 N4 2_556 . 2_555 85.1(19) ?
N4 I6 N4 1_556 . 2_555 100(2) ?
Pb1 I7 Pb1 . . 2_555 167.2(7) ?
Pb1 I7 N3 . . . 80.7(13) ?
Pb1 I7 N3 . . 2_555 110.7(13) ?
Pb1 I7 N3 2_555 . . 110.7(13) ?
Pb1 I7 N3 2_555 . 2_555 80.7(13) ?
N3 I7 N3 . . 2_555 60.4(18) ?
Pb1 I9 Pb1 . . 2_556 179.6(7) ?
Pb1 I10 Pb1 . . 2_655 179.6(7) ?
Pb1 I11 Pb1 . . 2_656 167.6(6) ?
Pb1 I11 N2 . . . 92.1(11) ?
Pb1 I11 N2 . . 2_656 99.5(11) ?
Pb1 I11 N2 2_656 . . 99.5(11) ?
Pb1 I11 N2 2_656 . 2_656 92.1(11) ?
N2 I11 N2 . . 2_656 42.8(15) ?

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
? ? ? ? ? ? ? ? ? ? ?


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Hydriodic Acid'
####################################################################### 
# 
# 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_I_CCDC5
_database_code_depnum_ccdc_archive 'CCDC 2018081'
loop_
_audit_author_name
_audit_author_address
'Justin M. Hoffman'
;Northwestern University
United States of America
;
_audit_update_record             
;
2020-09-18 deposited with the CCDC.	2020-10-06 downloaded from the CCDC.
;
#=======================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic        'IAA n = 2'
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_iupac          ?
_chemical_formula_weight         1314.7
_chemical_melting_point          ?
_chemical_compound_source        ?
_chemical_absolute_configuration ?

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

# 6. CRYSTAL DATA

_symmetry_cell_setting           monoclinic
_space_group_ssg_name            P2(\a0\g)0

loop_
_space_group_symop_ssg_id
_space_group_symop_ssg_operation_algebraic
1 x1,x2,x3,x4
2 -x1,x2,-x3,-x4

_cell_length_a                   8.8957(4)
_cell_length_b                   42.8038(19)
_cell_length_c                   8.9021(4)
_cell_angle_alpha                90
_cell_angle_beta                 89.326(3)
_cell_angle_gamma                90
_cell_volume                     3389.4(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
? ? ? ? ? ? ? ? ? ? ?


_cell_modulation_dimension       1
loop_
_cell_wave_vector_seq_id
_cell_wave_vector_x
_cell_wave_vector_y
_cell_wave_vector_z
1 0.125000 0.000000 0.125000

_jana_cell_commen_supercell_matrix_1_1 8
_jana_cell_commen_supercell_matrix_1_2 0
_jana_cell_commen_supercell_matrix_1_3 0
_jana_cell_commen_supercell_matrix_2_1 0
_jana_cell_commen_supercell_matrix_2_2 1
_jana_cell_commen_supercell_matrix_2_3 0
_jana_cell_commen_supercell_matrix_3_1 0
_jana_cell_commen_supercell_matrix_3_2 0
_jana_cell_commen_supercell_matrix_3_3 8
_jana_cell_commen_t_section_1    0

_cell_formula_units_Z            4

_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?
_cell_measurement_temperature    273
_cell_special_details            
; ?
;

_exptl_crystal_density_diffrn    2.5764
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             2140

_exptl_absorpt_coefficient_mu    16.277
_exptl_crystal_description       plate
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_exptl_crystal_size_rad          ?
_exptl_crystal_colour            red
_exptl_absorpt_correction_type   Gaussian
_exptl_absorpt_process_details   Jana2006
_exptl_absorpt_correction_T_min  0.173
_exptl_absorpt_correction_T_max  0.3321
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2 17 30 0.06418
-1 -6 -30 0.06561
0 1 0 0.04354
-1 -30 0 0.04396
30 -19 -5 0.06324
-5 3 0 0.07

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

# 7. EXPERIMENTAL DATA

_exptl_special_details           ?

_diffrn_ambient_temperature      298
_diffrn_source                   
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_power             2.00
_diffrn_source_voltage           50
_diffrn_source_current           40
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker CCD'
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            CCD
_diffrn_measurement_method       'Bruker CCD'
_diffrn_measurement_specimen_support ?

_diffrn_reflns_number            15762
_diffrn_reflns_theta_min         0.95
_diffrn_reflns_theta_max         29.08
_diffrn_reflns_theta_full        11.51
_diffrn_measured_fraction_theta_max 0.2
_diffrn_measured_fraction_theta_full 0.97
_diffrn_reflns_av_R_equivalents  0.07
_diffrn_reflns_av_unetI/netI     0.1014
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_k_max       50
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_index_m_1_min -1
_diffrn_reflns_limit_index_m_1_max 1
_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             7455
_reflns_number_gt                2686
_reflns_threshold_expression     I>2σ(I)

_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_gt           0.0963
_refine_ls_wR_factor_gt          0.1737
_refine_ls_R_factor_all          0.2302
_refine_ls_wR_factor_ref         0.1895
_refine_ls_goodness_of_fit_ref   2.25
_refine_ls_goodness_of_fit_gt    3.67
_refine_ls_restrained_S_gt       ?
_refine_ls_restrained_S_all      ?
_refine_ls_number_reflns         7455
_refine_ls_number_parameters     496
_refine_ls_number_restraints     0
_refine_ls_number_constraints    1
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     w=1/(σ²(I)+0.0004I²)
_refine_ls_hydrogen_treatment    ?
_refine_ls_shift/su_max          0.0320
_refine_ls_shift/su_mean         0.0207
_refine_diff_density_max         2.70
_refine_diff_density_min         -2.97
_refine_ls_extinction_method     
'B-C type 1 Gaussian isotropic (Becker & Coppens, 1974)'
_refine_ls_extinction_coef       5800(200)
_refine_ls_extinction_expression ?
_refine_ls_abs_structure_details 
;  2283 of Friedel pairs used in the refinement
;
_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 0.0033 0.0016 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
I -0.4742 1.8119 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
Pb -3.3944 10.1111 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'

_computing_data_collection       'STOE X-AREA'
_computing_cell_refinement       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_solution    ?
_computing_structure_refinement  ?
_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
? ? ? ? ? ?

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
? ? ? ? ? ? ? ?

loop_
_restr_torsion_atom_site_label_1
_restr_torsion_site_symmetry_1
_restr_torsion_atom_site_label_2
_restr_torsion_site_symmetry_2
_restr_torsion_atom_site_label_3
_restr_torsion_site_symmetry_3
_restr_torsion_atom_site_label_4
_restr_torsion_site_symmetry_4
_restr_torsion_angle_target
_restr_torsion_weight_param
? ? ? ? ? ? ? ? ? ?

loop_
_restr_equal_distance_atom_site_label_1
_restr_equal_distance_site_symmetry_1
_restr_equal_distance_atom_site_label_2
_restr_equal_distance_site_symmetry_2
_restr_equal_distance_class_class_id
_restr_equal_distance_class_target_weight_param
? ? ? ? ? ?

loop_
_restr_equal_angle_atom_site_label_1
_restr_equal_angle_site_symmetry_1
_restr_equal_angle_atom_site_label_2
_restr_equal_angle_site_symmetry_2
_restr_equal_angle_atom_site_label_3
_restr_equal_angle_site_symmetry_3
_restr_equal_angle_class_class_id
_restr_equal_angle_class_target_weight_param
? ? ? ? ? ? ? ?

loop_
_restr_equal_torsion_atom_site_label_1
_restr_equal_torsion_site_symmetry_1
_restr_equal_torsion_atom_site_label_2
_restr_equal_torsion_site_symmetry_2
_restr_equal_torsion_atom_site_label_3
_restr_equal_torsion_site_symmetry_3
_restr_equal_torsion_atom_site_label_4
_restr_equal_torsion_site_symmetry_4
_restr_equal_torsion_class_class_id
_restr_equal_torsion_class_target_weight_param
? ? ? ? ? ? ? ? ? ?


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

# 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 0.7500(4) -0.2918(3) -0.2501(4) Uani 0.089(4) 2 1 d . . .
Pb2 Pb 0.2509(4) -0.7927(3) -0.2503(4) Uani 0.071(3) 2 1 d . . .
Pb3 Pb 0.7495(5) -0.1402(3) -0.2497(4) Uani 0.076(3) 2 1 d . . .
Pb4 Pb 0.2504(4) -0.6410(3) -0.2489(4) Uani 0.066(3) 2 1 d . . .
I1 I 0 -0.2919(5) -0.5 Uani 0.148(9) 1 1 d . . .
I2 I 0.5 -0.2877(5) 0 Uani 0.144(9) 1 1 d . . .
I3 I 0 -0.2854(4) 0 Uani 0.124(8) 1 1 d . . .
I4 I 0.5 -0.2920(6) -0.5 Uani 0.39(2) 1 1 d . . .
I5 I 0.7441(8) -0.2162(4) -0.2638(7) Uani 0.182(5) 2 1 d . . .
I6 I 0 -0.7801(3) -0.5 Uani 0.084(6) 1 1 d . . .
I7 I 0.5 -0.8037(4) 0 Uani 0.143(8) 1 1 d . . .
I8 I 0.7628(12) -0.3644(4) -0.2231(11) Uani 0.217(8) 2 1 d . . .
I9 I 0.7545(14) -0.0701(4) -0.2344(12) Uani 0.272(9) 2 1 d . . .
I10 I 0.5 -0.1416(4) 0 Uani 0.127(8) 1 1 d . . .
I11 I 0 -0.7945(5) 0 Uani 0.152(10) 1 1 d . . .
I12 I 0 -0.1392(5) -0.5 Uani 0.150(9) 1 1 d . . .
I13 I 0.2836(6) -0.7170(4) -0.2122(5) Uani 0.079(3) 2 1 d . . .
I15 I 0.5 -0.7895(4) -0.5 Uani 0.104(8) 1 1 d . . .
I18 I 0.2124(9) -0.8638(4) -0.2994(8) Uani 0.091(5) 2 1 d . . .
I20 I 0 -0.6435(4) 0 Uani 0.093(7) 1 1 d . . .
I21 I 0.5 -0.6426(4) -0.5 Uani 0.143(9) 1 1 d . . .
I22 I 1 -0.1474(6) 0 Uani 0.349(18) 1 1 d . . .
I23 I 0.5 -0.1401(4) -0.5 Uani 0.130(8) 1 1 d . . .
I24 I 0.2024(9) -0.5697(3) -0.2950(9) Uani 0.098(5) 2 1 d . . .
I25 I 0.5 -0.6316(4) 0 Uani 0.099(7) 1 1 d . . .
I26 I 0 -1(2) -0.5 Uani 0.097(6) 1 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
? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ?


loop_
_atom_site_Fourier_wave_vector_seq_id
_jana_atom_site_Fourier_wave_vector_q1_coeff
1 1

loop_
_jana_atom_site_crenel_ortho_func_id
_jana_atom_site_crenel_ortho_func_c
_jana_atom_site_crenel_ortho_func_w
_jana_atom_site_crenel_ortho_func_eps
? ? ? ?

loop_
_jana_atom_site_occ_Fourier_absolute_site_label
_jana_atom_site_occ_Fourier_absolute
? ?

loop_
_atom_site_occ_Fourier_atom_site_label
_atom_site_occ_Fourier_wave_vector_seq_id
_atom_site_occ_Fourier_param_cos
_atom_site_occ_Fourier_param_sin
? ? ? ?

loop_
_jana_atom_site_occ_Legendre_atom_site_label
_jana_atom_site_occ_Legendre_param_order
_jana_atom_site_occ_Legendre_param_coeff
? ? ?

loop_
_jana_atom_site_occ_XHarm_atom_site_label
_jana_atom_site_occ_XHarm_param_order
_jana_atom_site_occ_XHarm_param_coeff
? ? ?

loop_
_jana_atom_site_occ_crenel_ortho_atom_site_label
_jana_atom_site_occ_crenel_ortho_param_order
_jana_atom_site_occ_crenel_ortho_id
_jana_atom_site_occ_crenel_ortho_param_coeff
? ? ? ?

loop_
_atom_site_occ_special_func_atom_site_label
_atom_site_occ_special_func_crenel_c
_atom_site_occ_special_func_crenel_w
? ? ?

loop_
_atom_site_displace_Fourier_atom_site_label
_atom_site_displace_Fourier_axis
_atom_site_displace_Fourier_wave_vector_seq_id
_atom_site_displace_Fourier_param_cos
_atom_site_displace_Fourier_param_sin
Pb1 x 1 0.0010(8) -0.0064(10)
Pb1 y 1 0.0090(2) 0.0000(2)
Pb1 z 1 0.0000(9) 0.0051(11)
Pb2 x 1 0.0011(7) 0.0054(9)
Pb2 y 1 -0.0095(2) 0.0000(2)
Pb2 z 1 0.0003(8) -0.0044(11)
I1 x 1 0 0.001(3)
I1 y 1 0.0110(6) 0
I1 z 1 0 0.004(3)
I2 x 1 0 -0.005(3)
I2 y 1 0.0119(6) 0
I2 z 1 0 -0.011(3)
I3 x 1 0 -0.002(2)
I3 y 1 0.0076(6) 0
I3 z 1 0 0.002(2)
I4 x 1 0 0.004(3)
I4 y 1 0.0049(11) 0
I4 z 1 0 -0.016(3)
I5 x 1 0.001(2) 0.011(3)
I5 y 1 0.0095(4) 0.0002(3)
I5 z 1 -0.003(2) 0.004(2)
I6 x 1 0 0.0075(18)
I6 y 1 -0.0087(5) 0
I6 z 1 0 -0.004(2)
I7 x 1 0 -0.010(2)
I7 y 1 -0.0090(5) 0
I7 z 1 0 0.013(3)
I8 x 1 -0.005(2) -0.016(2)
I8 y 1 0.0104(5) 0.0003(4)
I8 z 1 -0.004(2) 0.023(2)
I9 x 1 0.002(3) 0.020(3)
I9 y 1 0.0069(5) -0.0006(4)
I9 z 1 0.004(2) -0.014(3)
Pb3 x 1 0.0014(9) 0.0043(10)
Pb3 y 1 0.0092(2) 0.0002(2)
Pb3 z 1 -0.0003(8) -0.0061(9)
I10 x 1 0 0.003(2)
I10 y 1 0.0071(6) 0
I10 z 1 0 -0.007(2)
I11 x 1 0 -0.015(3)
I11 y 1 -0.0086(6) 0
I11 z 1 0 -0.010(2)
I12 x 1 0 0.009(3)
I12 y 1 0.0088(6) 0
I12 z 1 0 -0.011(3)
Pb4 x 1 0.0009(8) -0.0052(10)
Pb4 y 1 -0.0096(2) -0.0001(2)
Pb4 z 1 -0.0008(8) 0.0092(10)
I13 x 1 -0.0031(18) -0.0119(19)
I13 y 1 -0.0099(3) 0.0000(3)
I13 z 1 0.0036(17) -0.0005(18)
I15 x 1 0 0.012(2)
I15 y 1 -0.0117(5) 0
I15 z 1 0 0.013(2)
I18 x 1 -0.0069(15) 0.0168(16)
I18 y 1 -0.0102(3) 0.0007(3)
I18 z 1 -0.0075(16) -0.0244(16)
I20 x 1 0 -0.001(2)
I20 y 1 -0.0100(5) 0
I20 z 1 0 0.015(2)
I21 x 1 0 -0.015(3)
I21 y 1 -0.0068(6) 0
I21 z 1 0 0.005(3)
I22 x 1 0 0.008(3)
I22 y 1 0.0063(10) 0
I22 z 1 0 -0.014(3)
I23 x 1 0 0.004(2)
I23 y 1 0.0088(6) 0
I23 z 1 0 -0.008(2)
I24 x 1 0.0079(16) -0.0229(16)
I24 y 1 -0.0086(3) -0.0001(4)
I24 z 1 0.0064(17) 0.0169(17)
I25 x 1 0 -0.001(2)
I25 y 1 -0.0117(5) 0
I25 z 1 0 0.011(2)
I26 x 1 0 -0.009(2)
I26 y 1 -0.0073(5) 0
I26 z 1 0 0.014(2)

loop_
_jana_atom_site_displace_Legendre_atom_site_label
_jana_atom_site_displace_Legendre_axis
_jana_atom_site_displace_Legendre_param_order
_jana_atom_site_displace_Legendre_param_coeff
? ? ? ?

loop_
_jana_atom_site_displace_XHarm_site_label
_jana_atom_site_displace_XHarm_axis
_jana_atom_site_displace_XHarm_param_order
_jana_atom_site_displace_XHarm_param_coeff
? ? ? ?

loop_
_jana_atom_site_displace_crenel_ortho_atom_site_label
_jana_atom_site_displace_crenel_ortho_axis
_jana_atom_site_displace_crenel_ortho_id
_jana_atom_site_displace_crenel_ortho_param_order
_jana_atom_site_displace_crenel_ortho_param_coeff
? ? ? ? ?

loop_
_atom_site_displace_special_func_atom_site_label
_atom_site_displace_special_func_sawtooth_ax
_atom_site_displace_special_func_sawtooth_ay
_atom_site_displace_special_func_sawtooth_az
_atom_site_displace_special_func_sawtooth_c
_atom_site_displace_special_func_sawtooth_w
? ? ? ? ? ?

loop_
_atom_site_U_Fourier_atom_site_label
_atom_site_U_Fourier_tens_elem
_atom_site_U_Fourier_wave_vector_seq_id
_atom_site_U_Fourier_param_cos
_atom_site_U_Fourier_param_sin
Pb1 U11 1 0.048(9) -0.020(7)
Pb1 U22 1 0.040(12) 0.002(10)
Pb1 U33 1 -0.036(10) 0.009(8)
Pb1 U12 1 -0.005(6) -0.003(8)
Pb1 U13 1 -0.008(6) 0.000(6)
Pb1 U23 1 0.001(7) -0.024(9)
Pb2 U11 1 -0.009(7) 0.006(6)
Pb2 U22 1 -0.076(10) 0.001(9)
Pb2 U33 1 -0.023(10) 0.003(8)
Pb2 U12 1 0.002(5) 0.003(6)
Pb2 U13 1 -0.028(6) 0.001(6)
Pb2 U23 1 -0.006(6) 0.010(8)
I1 U11 1 0.04(2) 0
I1 U22 1 0.01(3) 0
I1 U33 1 0.03(2) 0
I1 U12 1 0 -0.02(2)
I1 U13 1 0.047(16) 0
I1 U23 1 0 -0.06(2)
I2 U11 1 0.13(2) 0
I2 U22 1 0.01(2) 0
I2 U33 1 -0.04(2) 0
I2 U12 1 0 0.00(2)
I2 U13 1 0.045(16) 0
I2 U23 1 0 -0.07(2)
I3 U11 1 0.06(2) 0
I3 U22 1 0.04(3) 0
I3 U33 1 0.011(19) 0
I3 U12 1 0 0.023(18)
I3 U13 1 -0.006(14) 0
I3 U23 1 0 -0.03(2)
I4 U11 1 0.16(3) 0
I4 U22 1 -0.39(8) 0
I4 U33 1 -0.06(3) 0
I4 U12 1 0 -0.11(4)
I4 U13 1 -0.05(2) 0
I4 U23 1 0 -0.06(4)
I5 U11 1 0.01(3) 0.01(3)
I5 U22 1 0.01(2) -0.04(2)
I5 U33 1 -0.03(2) 0.05(2)
I5 U12 1 0.004(12) 0.006(14)
I5 U13 1 0.000(18) 0.049(17)
I5 U23 1 -0.015(11) -0.012(15)
I6 U11 1 -0.052(14) 0
I6 U22 1 -0.003(19) 0
I6 U33 1 -0.04(2) 0
I6 U12 1 0 -0.016(13)
I6 U13 1 0.012(13) 0
I6 U23 1 0 -0.044(17)
I7 U11 1 -0.07(2) 0
I7 U22 1 -0.02(3) 0
I7 U33 1 -0.07(3) 0
I7 U12 1 0 -0.059(16)
I7 U13 1 -0.042(17) 0
I7 U23 1 0 0.145(17)
I8 U11 1 0.00(2) 0.07(2)
I8 U22 1 0.04(2) 0.00(2)
I8 U33 1 -0.02(2) -0.03(2)
I8 U12 1 0.024(15) -0.066(18)
I8 U13 1 -0.043(17) -0.017(17)
I8 U23 1 0.001(15) 0.056(18)
I9 U11 1 0.02(3) 0.03(3)
I9 U22 1 0.02(2) 0.024(18)
I9 U33 1 0.00(3) -0.06(2)
I9 U12 1 -0.002(18) 0.027(19)
I9 U13 1 0.01(2) -0.03(2)
I9 U23 1 0.015(17) -0.096(18)
Pb3 U11 1 0.041(9) -0.020(9)
Pb3 U22 1 0.042(10) 0.004(9)
Pb3 U33 1 -0.027(8) 0.008(7)
Pb3 U12 1 0.004(6) -0.009(8)
Pb3 U13 1 0.007(6) 0.006(6)
Pb3 U23 1 0.003(6) -0.002(8)
I10 U11 1 0.03(2) 0
I10 U22 1 0.05(3) 0
I10 U33 1 -0.05(2) 0
I10 U12 1 0 0.01(2)
I10 U13 1 0.000(16) 0
I10 U23 1 0 0.02(2)
I11 U11 1 -0.07(2) 0
I11 U22 1 -0.07(3) 0
I11 U33 1 -0.03(2) 0
I11 U12 1 0 0.00(2)
I11 U13 1 -0.063(16) 0
I11 U23 1 0 -0.05(2)
I12 U11 1 0.01(3) 0
I12 U22 1 -0.02(3) 0
I12 U33 1 0.00(2) 0
I12 U12 1 0 0.01(2)
I12 U13 1 -0.019(18) 0
I12 U23 1 0 0.01(2)
Pb4 U11 1 -0.012(7) -0.001(7)
Pb4 U22 1 -0.083(9) 0.005(8)
Pb4 U33 1 -0.024(9) 0.001(8)
Pb4 U12 1 0.000(5) 0.001(7)
Pb4 U13 1 -0.022(5) 0.001(6)
Pb4 U23 1 -0.005(6) 0.003(8)
I13 U11 1 0.044(17) -0.014(15)
I13 U22 1 -0.058(14) 0.007(17)
I13 U33 1 -0.010(16) -0.018(15)
I13 U12 1 0.014(6) 0.001(9)
I13 U13 1 -0.020(12) -0.030(11)
I13 U23 1 0.011(7) -0.010(11)
I15 U11 1 -0.036(16) 0
I15 U22 1 -0.01(2) 0
I15 U33 1 -0.07(2) 0
I15 U12 1 0 0.001(16)
I15 U13 1 -0.070(14) 0
I15 U23 1 0 0.04(2)
I18 U11 1 0.002(14) 0.026(13)
I18 U22 1 -0.058(14) -0.018(15)
I18 U33 1 0.043(14) -0.018(13)
I18 U12 1 -0.022(9) 0.008(12)
I18 U13 1 -0.029(10) 0.000(10)
I18 U23 1 0.026(10) -0.018(12)
I20 U11 1 0.018(17) 0
I20 U22 1 -0.06(2) 0
I20 U33 1 -0.01(2) 0
I20 U12 1 0 0.011(15)
I20 U13 1 0.007(14) 0
I20 U23 1 0 0.036(17)
I21 U11 1 0.01(2) 0
I21 U22 1 -0.04(3) 0
I21 U33 1 0.03(2) 0
I21 U12 1 0 -0.05(2)
I21 U13 1 0.015(18) 0
I21 U23 1 0 -0.02(2)
I22 U11 1 0.07(4) 0
I22 U22 1 0.22(7) 0
I22 U33 1 -0.08(3) 0
I22 U12 1 0 -0.07(4)
I22 U13 1 0.01(2) 0
I22 U23 1 0 0.00(4)
I23 U11 1 0.02(2) 0
I23 U22 1 0.02(3) 0
I23 U33 1 -0.063(18) 0
I23 U12 1 0 -0.01(2)
I23 U13 1 0.035(14) 0
I23 U23 1 0 -0.008(19)
I24 U11 1 0.012(14) -0.026(13)
I24 U22 1 -0.064(13) -0.004(14)
I24 U33 1 0.040(15) 0.007(15)
I24 U12 1 0.015(9) -0.012(11)
I24 U13 1 -0.027(11) 0.014(10)
I24 U23 1 -0.015(10) 0.011(12)
I25 U11 1 0.009(16) 0
I25 U22 1 -0.04(2) 0
I25 U33 1 0.03(2) 0
I25 U12 1 0 0.021(14)
I25 U13 1 -0.037(14) 0
I25 U23 1 0 -0.085(17)
I26 U11 1 -0.02(2) 0
I26 U22 1 0.01(2) 0
I26 U33 1 -0.012(19) 0
I26 U12 1 0 0.016(14)
I26 U13 1 -0.065(14) 0
I26 U23 1 0 0.069(14)

loop_
_jana_atom_site_U_Legendre_atom_site_label
_jana_atom_site_U_Legendre_tens_elem
_jana_atom_site_U_Legendre_param_order
_jana_atom_site_U_Legendre_param_coeff
? ? ? ?

loop_
_jana_atom_site_U_XHarm_atom_site_label
_jana_atom_site_U_XHarm_tens_elem
_jana_atom_site_U_XHarm_param_order
_jana_atom_site_U_XHarm_param_coeff
? ? ? ?

loop_
_jana_atom_site_U_crenel_ortho_atom_site_label
_jana_atom_site_U_crenel_ortho_tens_elem
_jana_atom_site_U_crenel_ortho_id
_jana_atom_site_U_crenel_ortho_param_order
_jana_atom_site_U_crenel_ortho_param_coeff
? ? ? ? ?

loop_
_jana_atom_site_ADP_C_Fourier_atom_site_label
_jana_atom_site_ADP_C_Fourier_tens_elem
_jana_atom_site_ADP_C_Fourier_wave_vector_seq_id
_jana_atom_site_ADP_C_Fourier_param_cos
_jana_atom_site_ADP_C_Fourier_param_sin
? ? ? ? ?

loop_
_jana_atom_site_ADP_D_Fourier_atom_site_label
_jana_atom_site_ADP_D_Fourier_tens_elem
_jana_atom_site_ADP_D_Fourier_wave_vector_seq_id
_jana_atom_site_ADP_D_Fourier_param_cos
_jana_atom_site_ADP_D_Fourier_param_sin
? ? ? ? ?

loop_
_jana_atom_site_ADP_E_Fourier_atom_site_label
_jana_atom_site_ADP_E_Fourier_tens_elem
_jana_atom_site_ADP_E_Fourier_wave_vector_seq_id
_jana_atom_site_ADP_E_Fourier_param_cos
_jana_atom_site_ADP_E_Fourier_param_sin
? ? ? ? ?

loop_
_jana_atom_site_ADP_F_Fourier_atom_site_label
_jana_atom_site_ADP_F_Fourier_tens_elem
_jana_atom_site_ADP_F_Fourier_wave_vector_seq_id
_jana_atom_site_ADP_F_Fourier_param_cos
_jana_atom_site_ADP_F_Fourier_param_sin
? ? ? ? ?


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

# 10. MOLECULAR GEOMETRY


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_ssg_symmetry_1
_geom_bond_site_ssg_symmetry_2
_geom_bond_distance_av
_geom_bond_distance_min
_geom_bond_distance_max
_geom_bond_publ_flag
Pb1 I1 . 1_6555 3.172(15) 3.159(19) 3.185(19) ?
Pb1 I2 . . 3.185(14) 3.167(18) 3.203(18) ?
Pb1 I3 . 1_6555 3.149(14) 3.11(2) 3.19(2) ?
Pb1 I4 . . 3.191(15) 3.14(2) 3.24(2) ?
Pb1 I5 . . 3.26(3) 3.24(3) 3.27(3) ?
Pb1 I8 . . 3.13(3) 3.12(3) 3.15(3) ?
Pb2 I6 . . 3.184(16) 3.15(2) 3.21(2) ?
Pb2 I7 . . 3.155(18) 3.00(2) 3.31(2) ?
Pb2 I11 . . 3.141(18) 3.11(3) 3.17(3) ?
Pb2 I13 . . 3.26(3) 3.25(3) 3.28(3) ?
Pb2 I15 . . 3.135(16) 3.12(2) 3.15(2) ?
Pb2 I18 . . 3.11(3) 3.06(3) 3.15(3) ?
I5 Pb3 . . 3.30(3) 3.29(3) 3.31(3) ?
I9 Pb3 . . 3.08(3) 3.06(3) 3.09(3) ?
Pb3 I10 . . 3.204(15) 3.173(19) 3.235(19) ?
Pb3 I12 . 1_6555 3.144(15) 3.13(2) 3.16(2) ?
Pb3 I22 . . 3.181(15) 3.15(2) 3.22(2) ?
Pb3 I23 . . 3.157(14) 3.09(2) 3.23(2) ?
Pb4 I13 . . 3.22(3) 3.20(3) 3.25(3) ?
Pb4 I20 . . 3.119(16) 3.10(2) 3.14(2) ?
Pb4 I21 . . 3.150(18) 3.13(3) 3.17(3) ?
Pb4 I24 . . 3.04(3) 2.98(3) 3.10(3) ?
Pb4 I25 . . 3.188(16) 3.13(2) 3.25(2) ?
Pb4 I26 . . 3(3) 3(7) 3(7) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_ssg_symmetry_1
_geom_angle_site_ssg_symmetry_2
_geom_angle_site_ssg_symmetry_3
_geom_angle_av
_geom_angle_min
_geom_angle_max
_geom_angle_publ_flag
I1 Pb1 I2 1_6555 . . 178.5(8) 177.6(9) 179.2(7) ?
I1 Pb1 I3 1_6555 . 1_6555 90.9(5) 90.2(4) 91.6(4) ?
I1 Pb1 I4 1_6555 . . 89.6(5) 88.5(4) 90.6(4) ?
I1 Pb1 I5 1_6555 . . 91.9(6) 91.1(7) 92.6(7) ?
I1 Pb1 I8 1_6555 . . 90.7(7) 88.6(7) 92.8(7) ?
I2 Pb1 I3 . . 1_6555 89.9(5) 89.1(4) 90.6(4) ?
I2 Pb1 I4 . . . 89.7(5) 88.7(4) 90.6(4) ?
I2 Pb1 I5 . . . 87.6(7) 86.2(7) 89.0(7) ?
I2 Pb1 I8 . . . 89.8(6) 89.4(6) 90.2(6) ?
I3 Pb1 I4 1_6555 . . 177.9(8) 177.3(8) 179.1(9) ?
I3 Pb1 I5 1_6555 . . 88.4(6) 86.2(6) 90.6(6) ?
I3 Pb1 I8 1_6555 . . 92.1(6) 90.3(6) 93.9(6) ?
I4 Pb1 I5 . . . 90.1(7) 87.2(6) 92.9(6) ?
I4 Pb1 I8 . . . 89.5(6) 88.7(6) 90.2(6) ?
I5 Pb1 I8 . . . 176.4(5) 174.7(5) 179.1(5) ?
I6 Pb2 I7 . . . 177.7(8) 176.7(9) 178.3(8) ?
I6 Pb2 I11 . . . 89.7(6) 88.8(6) 90.9(6) ?
I6 Pb2 I13 . . . 88.3(7) 85.6(6) 91.1(7) ?
I6 Pb2 I15 . . . 89.6(5) 88.1(6) 91.2(5) ?
I6 Pb2 I18 . . . 89.5(7) 87.9(6) 91.1(7) ?
I7 Pb2 I11 . . . 90.1(6) 89.7(6) 90.3(6) ?
I7 Pb2 I13 . . . 89.6(8) 87.5(7) 91.9(7) ?
I7 Pb2 I15 . . . 90.4(5) 89.8(5) 91.2(5) ?
I7 Pb2 I18 . . . 92.6(8) 90.7(7) 94.4(8) ?
I11 Pb2 I13 . . . 88.2(8) 85.3(10) 91.1(10) ?
I11 Pb2 I15 . . . 174.9(10) 170.1(12) 179.5(6) ?
I11 Pb2 I18 . . . 94.0(8) 88.7(10) 99.2(10) ?
I13 Pb2 I15 . . . 86.8(7) 84.7(7) 88.8(7) ?
I13 Pb2 I18 . . . 175.9(7) 173.4(7) 179.2(7) ?
I15 Pb2 I18 . . . 91.0(8) 90.5(7) 91.6(8) ?
Pb1 I1 Pb1 1_4555 . 2_6565 160.1(10) 158.9(11) 161.5(11) ?
Pb1 I2 Pb1 . . 2_6555 159.1(10) 157.2(10) 161.2(11) ?
Pb1 I3 Pb1 1_4555 . 2_6555 174.6(9) 173.7(8) 176.0(12) ?
Pb1 I4 Pb1 . . 2_6565 175.4(8) 174.7(8) 177.4(13) ?
Pb1 I5 Pb3 . . . 164.1(6) 163.4(6) 164.9(6) ?
Pb2 I6 Pb2 . . 2_5565 174.4(9) 169.9(10) 178.9(9) ?
Pb2 I7 Pb2 . . 2_6555 177.4(8) 176.5(9) 178.8(3) ?
I5 Pb3 I9 . . . 177.0(5) 175.2(5) 179.1(5) ?
I5 Pb3 I10 . . . 86.1(6) 84.4(6) 87.7(6) ?
I5 Pb3 I12 . . 1_6555 88.8(6) 86.7(6) 90.9(6) ?
I5 Pb3 I22 . . . 89.2(6) 87.4(7) 91.0(6) ?
I5 Pb3 I23 . . . 88.1(6) 85.8(6) 90.5(6) ?
I9 Pb3 I10 . . . 91.1(6) 90.7(6) 91.4(6) ?
I9 Pb3 I12 . . 1_6555 94.1(7) 93.8(7) 94.5(7) ?
I9 Pb3 I22 . . . 90.8(6) 89.8(6) 91.7(6) ?
I9 Pb3 I23 . . . 91.9(6) 90.1(6) 93.8(6) ?
I10 Pb3 I12 . . 1_6555 174.6(9) 174.1(8) 175.3(9) ?
I10 Pb3 I22 . . . 89.4(5) 88.3(5) 90.6(5) ?
I10 Pb3 I23 . . . 89.7(5) 89.3(4) 90.0(4) ?
I12 Pb3 I22 1_6555 . . 90.1(5) 89.0(5) 91.0(5) ?
I12 Pb3 I23 1_6555 . . 90.6(5) 88.7(5) 92.3(5) ?
I22 Pb3 I23 . . . 176.9(9) 175.1(9) 178.4(8) ?
Pb3 I10 Pb3 . . 2_6555 156.4(10) 153.5(11) 159.4(11) ?
Pb2 I11 Pb2 . . 2_5555 174.4(13) 171.3(17) 177.0(10) ?
Pb3 I12 Pb3 1_4555 . 2_6565 166.2(10) 162.7(11) 170.4(11) ?
I13 Pb4 I20 . . . 88.0(7) 87.3(7) 88.7(7) ?
I13 Pb4 I21 . . . 87.3(7) 86.4(7) 88.3(7) ?
I13 Pb4 I24 . . . 177.8(7) 176.5(7) 179.5(7) ?
I13 Pb4 I25 . . . 88.8(6) 86.9(7) 90.7(7) ?
I13 Pb4 I26 . . . 100(1700) 100(1700) 100(1700) ?
I20 Pb4 I21 . . . 174.8(9) 173.8(9) 175.5(11) ?
I20 Pb4 I24 . . . 92.3(8) 90.9(9) 93.7(9) ?
I20 Pb4 I25 . . . 89.8(5) 88.8(6) 90.7(6) ?
I20 Pb4 I26 . . . 90(30) 89.7(7) 91.5(18) ?
I21 Pb4 I24 . . . 92.3(8) 90.6(10) 94.0(10) ?
I21 Pb4 I25 . . . 89.5(5) 87.4(7) 91.6(7) ?
I21 Pb4 I26 . . . 90(140) 90(140) 90(140) ?
I24 Pb4 I25 . . . 89.2(7) 87.9(7) 90.5(7) ?
I24 Pb4 I26 . . . 100(1700) 100(1700) 100(1700) ?
I25 Pb4 I26 . . . 200(1300) 200(1700) 200(600) ?
Pb2 I13 Pb4 . . . 174.8(9) 173.1(8) 176.5(8) ?
Pb2 I15 Pb2 . . 2_6565 168.5(11) 166.7(14) 170.9(14) ?
Pb4 I20 Pb4 . . 2_5555 177.0(10) 176.7(14) 177.3(9) ?
Pb4 I21 Pb4 . . 2_6565 170.3(12) 166.9(16) 174.6(16) ?
Pb3 I22 Pb3 . . 2_7555 176.3(8) 175.0(8) 179.8(13) ?
Pb3 I23 Pb3 . . 2_6565 175.6(10) 174.9(10) 177.3(13) ?
Pb4 I25 Pb4 . . 2_6555 177.9(9) 176.5(11) 179.0(7) ?
Pb4 I26 Pb4 . . 2_5565 0(3000) 0(3000) 0(3000) ?

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_ssg_symmetry_1
_geom_torsion_site_ssg_symmetry_2
_geom_torsion_site_ssg_symmetry_3
_geom_torsion_site_ssg_symmetry_4
_geom_torsion_av
_geom_torsion_min
_geom_torsion_max
? ? ? ? ? ? ? ? ? ? ?

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
? ? ? ? ? ? ? ? ? ? ?


# start Validation Reply Form
_vrf_GEOM003_I                   
;
PROBLEM: _geom_bond_distance is missing
RESPONSE: Distances and angles are reported in the CIF
and this information is listed under the ' _geom_bond_distance_av'
and '_geom_angle_av' loops. The name of these modulation-related parameters
is different than the ones used for standard structures and checkCIF does
not recognized them even though distances and angles are listed
;


####################################################################### 
# 
# 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_I_CCDC6
_database_code_depnum_ccdc_archive 'CCDC 2018083'
loop_
_audit_author_name
_audit_author_address
'Justin Hoffman'
;Northwestern University
United States of America
;
_audit_update_record             
;
2020-07-21 deposited with the CCDC.	2020-10-06 downloaded from the CCDC.
;
#=======================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic        
; ?
;
_chemical_name_common            ?
_chemical_formula_moiety         '2(C5 H14 N 1+), Pb I4 2-'
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_iupac          ?
_chemical_formula_sum            'C10 H28 I4 N2 Pb1'
_chemical_formula_weight         891.2
_chemical_melting_point          ?
_chemical_compound_source        ?
_chemical_absolute_configuration .

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

# 6. CRYSTAL DATA

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ycb'
_symmetry_Int_Tables_number      14

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,-z
4 x,-y+1/2,z+1/2

_cell_length_a                   16.5590(38)
_cell_length_b                   8.7623(14)
_cell_length_c                   8.7693(16)
_cell_angle_alpha                90
_cell_angle_beta                 105.3538(16)
_cell_angle_gamma                90
_cell_volume                     1227.0(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 0.34(2) 1 0 0 0 1 0 0 0 1
2 0.386(14) -1 0 0 -0.5 0 1 -0.5 1 0
3 0.276(14) -1 0 0 0.5 0 -1 -0.5 -1 0

_cell_formula_units_Z            2

_cell_measurement_reflns_used    2447
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      24.87
_cell_measurement_temperature    293
_cell_special_details            
; ?
;

_exptl_crystal_density_diffrn    2.4121
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             792

_exptl_absorpt_coefficient_mu    11.898
_exptl_crystal_description       plate
_exptl_crystal_size_max          0.2380
_exptl_crystal_size_mid          0.1115
_exptl_crystal_size_min          0.0755
_exptl_crystal_size_rad          ?
_exptl_crystal_colour            yellow
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   ?
_exptl_absorpt_correction_T_min  0.0766
_exptl_absorpt_correction_T_max  0.2170
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 6 0.0755
1 4 -30 0.0760
1 30 1 0.2333
-7 -30 1 0.2380
6 -1 0 0.1160
-30 -7 4 0.1070

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

# 7. EXPERIMENTAL DATA

_exptl_special_details           ?

_diffrn_ambient_temperature      293
_diffrn_source                   ?
_diffrn_source_power             ?
_diffrn_source_voltage           ?
_diffrn_source_current           ?
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'IPDS Stoe'
_diffrn_detector                 ?
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_method       '??integration method??'
_diffrn_measurement_specimen_support ?

_diffrn_reflns_number            11455
_diffrn_reflns_theta_min         2.55
_diffrn_reflns_theta_max         29.27
_diffrn_reflns_theta_full        29.27
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measured_fraction_theta_full 0.99
_diffrn_reflns_av_R_equivalents  0.1924
_diffrn_reflns_av_unetI/netI     0.1017
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       11
_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          
; The structure was refined based on the following considerations.
 The perovskite lattice was refined anisotropically without
 any constraints on the Pb and I atoms. The highly anisotropic shape of
 the thermal ellipsoids of coordinated iodide ions appears due to a high
 thermal motion relative to the Pb-I bond vector. It is typical for the
 halide perovskites structures at room temperature and therefore no 
 special treatment was used. All organic atoms were refined isotropically.
 Restraints were applied to the C-C and C-N bond lengths. Each cation was
 treated as having equivalent thermal parameters. Significant disorder 
 exists in the interlayer cations,  causing the atoms to move and destabilize the refinement. 
 The bond length restraints cannot account for the motion of the interlayer cations. 
 Therefore the cations were modeled manually based on reasonable
 bond length and bond angle parameters. 
;

_reflns_number_total             3105
_reflns_number_gt                1154
_reflns_threshold_expression     I>3σ(I)

_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_gt           0.0757
_refine_ls_wR_factor_gt          0.1835
_refine_ls_R_factor_all          0.1811
_refine_ls_wR_factor_ref         0.1967
_refine_ls_goodness_of_fit_ref   3.30
_refine_ls_goodness_of_fit_gt    5.11
_refine_ls_restrained_S_gt       ?
_refine_ls_restrained_S_all      ?
_refine_ls_number_reflns         3105
_refine_ls_number_parameters     46
_refine_ls_number_restraints     10
_refine_ls_number_constraints    61
_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          0.0417
_refine_ls_shift/su_mean         0.0041
_refine_diff_density_max         2.78
_refine_diff_density_min         -2.07
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_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 0.0033 0.0016 '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 -0.4742 1.8119 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
N 0.0061 0.0033 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
Pb -3.3944 10.1111 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  ?
_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
N1 . C1a . 1.5 0.001
C1a . C1b . 1.5 0.001
C1b . C1c . 1.5 0.001
C1c . C1d . 1.5 0.001
C1c . C1e . 1.5 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
N1 . C1a . C1b . 109.47 0.01
C1a . C1b . C1c . 109.47 0.01
C1b . C1c . C1d . 109.47 0.01
C1b . C1c . C1e . 109.47 0.01
C1d . C1c . C1e . 109.47 0.01

loop_
_restr_torsion_atom_site_label_1
_restr_torsion_site_symmetry_1
_restr_torsion_atom_site_label_2
_restr_torsion_site_symmetry_2
_restr_torsion_atom_site_label_3
_restr_torsion_site_symmetry_3
_restr_torsion_atom_site_label_4
_restr_torsion_site_symmetry_4
_restr_torsion_angle_target
_restr_torsion_weight_param
? ? ? ? ? ? ? ? ? ?

loop_
_restr_equal_distance_atom_site_label_1
_restr_equal_distance_site_symmetry_1
_restr_equal_distance_atom_site_label_2
_restr_equal_distance_site_symmetry_2
_restr_equal_distance_class_class_id
_restr_equal_distance_class_target_weight_param
? ? ? ? ? ?

loop_
_restr_equal_angle_atom_site_label_1
_restr_equal_angle_site_symmetry_1
_restr_equal_angle_atom_site_label_2
_restr_equal_angle_site_symmetry_2
_restr_equal_angle_atom_site_label_3
_restr_equal_angle_site_symmetry_3
_restr_equal_angle_class_class_id
_restr_equal_angle_class_target_weight_param
? ? ? ? ? ? ? ?

loop_
_restr_equal_torsion_atom_site_label_1
_restr_equal_torsion_site_symmetry_1
_restr_equal_torsion_atom_site_label_2
_restr_equal_torsion_site_symmetry_2
_restr_equal_torsion_atom_site_label_3
_restr_equal_torsion_site_symmetry_3
_restr_equal_torsion_atom_site_label_4
_restr_equal_torsion_site_symmetry_4
_restr_equal_torsion_class_class_id
_restr_equal_torsion_class_target_weight_param
? ? ? ? ? ? ? ? ? ?


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

# 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 0.5 0.5 0 Uani 0.0921(11) 2 1 d . . .
I1 I 0.70200(14) 0.4996(5) 0.1021(6) Uani 0.143(2) 4 1 d . . .
I2 I 0.5003(4) 0.1889(3) 0.1911(4) Uani 0.1217(15) 4 1 d . . .
N1 N 0.354(3) -0.083(6) 0.013(7) Uiso 0.293(16) 4 1 d . . .
C1b C 0.233(2) -0.025(6) -0.211(5) Uiso 0.293(16) 4 1 d . . .
C1a C 0.307(3) 0.041(5) -0.092(7) Uiso 0.293(16) 4 1 d . . .
C1d C 0.141(3) -0.054(8) -0.036(6) Uiso 0.293(16) 4 1 d . . .
C1c C 0.154(2) 0.029(4) -0.177(5) Uiso 0.293(16) 4 1 d . . .
C1e C 0.082(2) 0.000(9) -0.318(6) Uiso 0.293(16) 4 1 d . . .
H1c1b H 0.235851 -0.13482 -0.203982 Uiso 0.3511 4 1 d . . .
H2c1b H 0.234449 0.006014 -0.314907 Uiso 0.3511 4 1 d . . .
H1c1a H 0.288134 0.115535 -0.028539 Uiso 0.3511 4 1 d . . .
H2c1a H 0.343822 0.089442 -0.145598 Uiso 0.3511 4 1 d . . .
H1c1d H 0.087874 -0.024387 -0.019443 Uiso 0.3511 4 1 d . . .
H2c1d H 0.140382 -0.162149 -0.055386 Uiso 0.3511 4 1 d . . .
H3c1d H 0.184933 -0.029633 0.05546 Uiso 0.3511 4 1 d . . .
H1c1c H 0.158181 0.136849 -0.15511 Uiso 0.3511 4 1 d . . .
H1c1e H 0.030487 -0.000615 -0.285955 Uiso 0.3511 4 1 d . . .
H2c1e H 0.079116 0.078574 -0.39527 Uiso 0.3511 4 1 d . . .
H3c1e H 0.088834 -0.097364 -0.363202 Uiso 0.3511 4 1 d . . .
H1n1 H 0.394004 -0.043581 0.086847 Uiso 0.3511 4 1 d . . .
H2n1 H 0.319393 -0.131665 0.056097 Uiso 0.3511 4 1 d . . .
H3n1 H 0.374382 -0.146548 -0.042901 Uiso 0.3511 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 . . 3.226(2) ?
Pb1 I1 . 3_665 3.226(2) ?
Pb1 I2 . . 3.199(4) ?
Pb1 I2 . 2_655 3.176(3) ?
Pb1 I2 . 3_665 3.199(4) ?
Pb1 I2 . 4_554 3.176(3) ?
I1 N1 . 2_655 3.80(6) ?
I1 N1 . 3_655 3.83(6) ?
I2 N1 . . 3.47(5) ?
I2 N1 . 2_655 3.64(5) ?
I2 N1 . 3_655 3.49(6) ?

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 . . 3_665 180.0(5) ?
I1 Pb1 I2 . . . 89.76(14) ?
I1 Pb1 I2 . . 2_655 89.98(14) ?
I1 Pb1 I2 . . 3_665 90.24(14) ?
I1 Pb1 I2 . . 4_554 90.02(14) ?
I1 Pb1 I2 3_665 . . 90.24(14) ?
I1 Pb1 I2 3_665 . 2_655 90.02(14) ?
I1 Pb1 I2 3_665 . 3_665 89.76(14) ?
I1 Pb1 I2 3_665 . 4_554 89.98(14) ?
I2 Pb1 I2 . . 2_655 89.86(8) ?
I2 Pb1 I2 . . 3_665 180.0(5) ?
I2 Pb1 I2 . . 4_554 90.14(8) ?
I2 Pb1 I2 2_655 . 3_665 90.14(8) ?
I2 Pb1 I2 2_655 . 4_554 180.0(5) ?
I2 Pb1 I2 3_665 . 4_554 89.86(8) ?
Pb1 I1 N1 . . 2_655 76.7(8) ?
Pb1 I1 N1 . . 3_655 76.6(8) ?
N1 I1 N1 2_655 . 3_655 87.4(12) ?
Pb1 I2 Pb1 . . 2_645 152.97(11) ?
Pb1 I2 N1 . . . 116.5(9) ?
Pb1 I2 N1 . . 2_655 79.3(9) ?
Pb1 I2 N1 . . 3_655 82.1(9) ?
Pb1 I2 N1 2_645 . . 82.3(10) ?
Pb1 I2 N1 2_645 . 2_655 80.1(9) ?
Pb1 I2 N1 2_645 . 3_655 117.2(9) ?
N1 I2 N1 . . 2_655 162.3(14) ?
N1 I2 N1 . . 3_655 94.9(13) ?
N1 I2 N1 2_655 . 3_655 95.2(13) ?

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
? ? ? ? ? ? ? ? ? ? ?


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Hydriodic Acid'
####################################################################### 
# 
# 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_I_CCDC7
_database_code_depnum_ccdc_archive 'CCDC 2018084'
loop_
_audit_author_name
_audit_author_address
'Justin Hoffman'
;Northwestern University
United States of America
;
_audit_update_record             
;
2020-07-21 deposited with the CCDC.	2020-10-06 downloaded from the CCDC.
;
#=======================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic        
; ?
;
_chemical_name_common            ?
_chemical_formula_moiety         '2(C4 H12 N 1+), 3(C H6 N 1+), Pb4 I13 5-'
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_iupac          ?
_chemical_formula_sum            'C11 H42 I13 N5 Pb4'
_chemical_formula_weight         2723
_chemical_melting_point          ?
_chemical_compound_source        ?
_chemical_absolute_configuration .

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

# 6. CRYSTAL DATA

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_Int_Tables_number      15

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

_cell_length_a                   8.9397(6)
_cell_length_b                   8.9386(7)
_cell_length_c                   63.648(4)
_cell_angle_alpha                90
_cell_angle_beta                 90.015(6)
_cell_angle_gamma                90
_cell_volume                     5086(2)

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 0.661(11) 1 0 0 0 1 0 0 0 1
2 0.339(11) 0 -1 0 -1 0 0 0 0 -1

_cell_formula_units_Z            4

_cell_measurement_reflns_used    21792
_cell_measurement_theta_min      2.28
_cell_measurement_theta_max      29.23
_cell_measurement_temperature    293
_cell_special_details            
; ?
;

_exptl_crystal_density_diffrn    3.5562
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             4632

_exptl_absorpt_coefficient_mu    21.104
_exptl_crystal_description       plate
_exptl_crystal_size_max          0.1472
_exptl_crystal_size_mid          0.0905
_exptl_crystal_size_min          0.0691
_exptl_crystal_size_rad          ?
_exptl_crystal_colour            black
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   ?
_exptl_absorpt_correction_T_min  0.0338
_exptl_absorpt_correction_T_max  0.1348
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
30 26 -15 0.1113
30 -19 -5 0.0979
2 1 -30 0.0691
3 2 -30 0.0723
1 30 -10 0.1345
0 0 1 0.0703
-30 5 11 0.1009
-7 -5 15 0.0905
-2 1 -30 0.1042
-30 17 2 0.0949
-1 2 30 0.0896
-1 0 10 0.0904
-1 -15 2 0.1472
0 -1 -15 0.0926
0 0 -1 0.0698

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

# 7. EXPERIMENTAL DATA

_exptl_special_details           ?

_diffrn_ambient_temperature      293
_diffrn_source                   ?
_diffrn_source_power             ?
_diffrn_source_voltage           ?
_diffrn_source_current           ?
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'IPDS Stoe'
_diffrn_detector                 ?
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_method       '??integration method??'
_diffrn_measurement_specimen_support ?

_diffrn_reflns_number            19314
_diffrn_reflns_theta_min         1.92
_diffrn_reflns_theta_max         29.24
_diffrn_reflns_theta_full        29.24
_diffrn_measured_fraction_theta_max 0.94
_diffrn_measured_fraction_theta_full 0.94
_diffrn_reflns_av_R_equivalents  0.3699
_diffrn_reflns_av_unetI/netI     0.7948
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -85
_diffrn_reflns_limit_l_max       86
_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          
; The structure was refined based on the following considerations.
 The perovskite lattice was refined anisotropically without
 any constraints on the Pb and I atoms. The highly anisotropic shape of
 the thermal ellipsoids of coordinated iodide ions appears due to a high
 thermal motion relative to the Pb-I bond vector. It is typical for the
 halide perovskites structures at room temperature and therefore no 
 special treatment was used. All organic atoms were refined isotropically.
 Restraints were applied to the C-C and C-N bond lengths. Each cation was
 treated as having equivalent thermal parameters. Significant disorder 
 exists in the interlayer cations,  causing the atoms to move and destabilize the refinement. 
 The bond length restraints cannot account for the motion of the interlayer cations. 
 Therefore the cations were modeled manually based on reasonable
 bond length and bond angle parameters.  Furthermore,
 as the crystal often co-precipitates with other n values, particularly n = 3,
 this structure had other phases grown on its surface, leading to a large amount
 of the data being discluded, leading to a low ratio of observed/unique reflections.
 Some of these cations are shown unreasonably close to one another due to this disorder.
 Furthermore, as the crystal often co-precipitates with other n values,
 this structure had other phases grown on its surface, leading to a large amount
 of the data being discluded, leading to a low ratio of observed/unique reflections.
;

_reflns_number_total             6873
_reflns_number_gt                752
_reflns_threshold_expression     I>3σ(I)

_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_gt           0.0980
_refine_ls_wR_factor_gt          0.1804
_refine_ls_R_factor_all          0.4058
_refine_ls_wR_factor_ref         0.2094
_refine_ls_goodness_of_fit_ref   1.30
_refine_ls_goodness_of_fit_gt    3.61
_refine_ls_restrained_S_gt       ?
_refine_ls_restrained_S_all      ?
_refine_ls_number_reflns         6873
_refine_ls_number_parameters     105
_refine_ls_number_restraints     10
_refine_ls_number_constraints    98
_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          0.0478
_refine_ls_shift/su_mean         0.0059
_refine_diff_density_max         4.45
_refine_diff_density_min         -2.41
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_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 0.0033 0.0016 '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 -0.4742 1.8119 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
N 0.0061 0.0033 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
Pb -3.3944 10.1111 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  ?
_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
N2 . C2a . 1.5 0.001
C2a . C2b . 1.5 0.001
C2b . C2c . 1.5 0.001
C2b . C2d . 1.5 0.001
N4 . C4 . 1.5 0.001
N1 . C1 . 1.5 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
N2 . C2a . C2b . 109.47 0.01
C2a . C2b . C2c . 109.47 0.01
C2a . C2b . C2d . 109.47 0.01
C2c . C2b . C2d . 109.47 0.01

loop_
_restr_torsion_atom_site_label_1
_restr_torsion_site_symmetry_1
_restr_torsion_atom_site_label_2
_restr_torsion_site_symmetry_2
_restr_torsion_atom_site_label_3
_restr_torsion_site_symmetry_3
_restr_torsion_atom_site_label_4
_restr_torsion_site_symmetry_4
_restr_torsion_angle_target
_restr_torsion_weight_param
? ? ? ? ? ? ? ? ? ?

loop_
_restr_equal_distance_atom_site_label_1
_restr_equal_distance_site_symmetry_1
_restr_equal_distance_atom_site_label_2
_restr_equal_distance_site_symmetry_2
_restr_equal_distance_class_class_id
_restr_equal_distance_class_target_weight_param
? ? ? ? ? ?

loop_
_restr_equal_angle_atom_site_label_1
_restr_equal_angle_site_symmetry_1
_restr_equal_angle_atom_site_label_2
_restr_equal_angle_site_symmetry_2
_restr_equal_angle_atom_site_label_3
_restr_equal_angle_site_symmetry_3
_restr_equal_angle_class_class_id
_restr_equal_angle_class_target_weight_param
? ? ? ? ? ? ? ?

loop_
_restr_equal_torsion_atom_site_label_1
_restr_equal_torsion_site_symmetry_1
_restr_equal_torsion_atom_site_label_2
_restr_equal_torsion_site_symmetry_2
_restr_equal_torsion_atom_site_label_3
_restr_equal_torsion_site_symmetry_3
_restr_equal_torsion_atom_site_label_4
_restr_equal_torsion_site_symmetry_4
_restr_equal_torsion_class_class_id
_restr_equal_torsion_class_target_weight_param
? ? ? ? ? ? ? ? ? ?


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

# 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 0.4992(5) 0.2465(5) 0.20028(5) Uani 0.0588(18) 8 1 d . . .
Pb2 Pb 0.4996(4) 0.2459(6) 0.10004(4) Uani 0.060(2) 8 1 d . . .
I1 I 0.2512(13) -0.0006(10) 0.1012(3) Uani 0.144(10) 8 1 d . . .
I2 I 0.7483(16) -0.0006(10) 0.1014(3) Uani 0.159(11) 8 1 d . . .
I3 I 0.2505(16) 0.0007(12) 0.1999(3) Uani 0.147(11) 8 1 d . . .
I4 I 0.4964(10) 0.2294(15) 0.15147(8) Uani 0.175(7) 8 1 d . . .
I5 I 0.2503(14) 0.5007(12) 0.2006(3) Uani 0.137(10) 8 1 d . . .
I6 I 0.5 0.228(2) 0.25 Uani 0.184(11) 4 1 d . . .
I7 I 0.4960(13) 0.1979(11) 0.05243(9) Uani 0.202(8) 8 1 d . . .
N1 N 0.5 -0.186(6) 0.25 Uiso 0.09(2) 4 1 d . . .
C2b C 0.497(4) -0.146(4) 0.0142(5) Uiso 0.107(14) 8 1 d . . .
C2c C 0.536(6) -0.218(7) -0.0063(5) Uiso 0.107(14) 8 1 d . . .
N4 N 0.427(5) -0.171(5) 0.1473(6) Uiso 0.055(11) 8 1 d . . .
C4 C 0.583(4) -0.197(5) 0.1551(8) Uiso 0.055(11) 8 1 d . . .
C2a C 0.565(4) -0.233(5) 0.0319(5) Uiso 0.107(14) 8 1 d . . .
N2 N 0.500(7) -0.181(8) 0.0524(5) Uiso 0.107(14) 8 1 d . . .
C2d C 0.330(4) -0.144(7) 0.0167(7) Uiso 0.107(14) 8 1 d . . .
C1 C 0.5 -0.019(6) 0.25 Uiso 0.09(2) 4 1 d . . .
H1c2b H 0.534029 -0.045119 0.014387 Uiso 0.1284 8 1 d . . .
H1c2c H 0.619895 -0.167293 -0.012456 Uiso 0.1284 8 1 d . . .
H2c2c H 0.561524 -0.321195 -0.003955 Uiso 0.1284 8 1 d . . .
H3c2c H 0.452031 -0.212556 -0.01568 Uiso 0.1284 8 1 d . . .
H1c4 H 0.584019 -0.284162 0.16398 Uiso 0.0657 8 1 d . . .
H2c4 H 0.648656 -0.213454 0.143352 Uiso 0.0657 8 1 d . . .
H3c4 H 0.616381 -0.111958 0.162919 Uiso 0.0657 8 1 d . . .
H1c2a H 0.544968 -0.337317 0.030017 Uiso 0.1284 8 1 d . . .
H2c2a H 0.671612 -0.216812 0.031985 Uiso 0.1284 8 1 d . . .
H1c2d H 0.287633 -0.069632 0.007548 Uiso 0.1284 8 1 d . . .
H2c2d H 0.289868 -0.240219 0.013259 Uiso 0.1284 8 1 d . . .
H3c2d H 0.305137 -0.119704 0.031025 Uiso 0.1284 8 1 d . . .
H1c1 H 0.404012 0.017155 0.254519 Uiso 0.1041 8 0.5 d . . .
H2c1 H 0.57588 0.017155 0.259417 Uiso 0.1041 8 0.5 d . . .
H3c1 H 0.520108 0.017155 0.236064 Uiso 0.1041 8 0.5 d . . .
H1n1 H 0.411491 -0.218897 0.2466 Uiso 0.1041 8 0.5 d . . .
H2n1 H 0.565197 -0.218897 0.240935 Uiso 0.1041 8 0.5 d . . .
H3n1 H 0.523312 -0.218897 0.262465 Uiso 0.1041 8 0.5 d . . .
H1n4 H 0.366625 -0.235186 0.152937 Uiso 0.0657 8 1 d . . .
H2n4 H 0.425076 -0.180499 0.133656 Uiso 0.0657 8 1 d . . .
H1n2 H 0.527003 -0.242173 0.062322 Uiso 0.1284 8 1 d . . .
H2n2 H 0.532762 -0.091648 0.055201 Uiso 0.1284 8 1 d . . .
H3n2 H 0.403157 -0.179633 0.051431 Uiso 0.1284 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 I3 . . 3.126(14) ?
Pb1 I3 . 5_555 3.195(14) ?
Pb1 I4 . . 3.110(6) ?
Pb1 I5 . . 3.181(13) ?
Pb1 I5 . 5_545 3.140(13) ?
Pb1 I6 . . 3.169(3) ?
Pb2 I1 . . 3.129(11) ?
Pb2 I1 . 5_555 3.194(11) ?
Pb2 I2 . . 3.131(13) ?
Pb2 I2 . 5_455 3.192(13) ?
Pb2 I4 . . 3.277(6) ?
Pb2 I7 . . 3.061(6) ?
I1 N4 . . 3.66(4) ?
I4 N4 . . 3.64(5) ?
I6 N1 . . 3.71(6) ?
I7 N2 . . 3.39(7) ?

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
I3 Pb1 I3 . . 5_555 178.9(4) ?
I3 Pb1 I4 . . . 87.2(4) ?
I3 Pb1 I5 . . . 90.2(3) ?
I3 Pb1 I5 . . 5_545 91.0(3) ?
I3 Pb1 I6 . . . 88.5(4) ?
I3 Pb1 I4 5_555 . . 91.9(4) ?
I3 Pb1 I5 5_555 . . 89.1(3) ?
I3 Pb1 I5 5_555 . 5_545 89.7(3) ?
I3 Pb1 I6 5_555 . . 92.5(4) ?
I4 Pb1 I5 . . . 92.0(4) ?
I4 Pb1 I5 . . 5_545 88.7(4) ?
I4 Pb1 I6 . . . 174.2(5) ?
I5 Pb1 I5 . . 5_545 178.6(4) ?
I5 Pb1 I6 . . . 91.9(4) ?
I5 Pb1 I6 5_545 . . 87.5(4) ?
I1 Pb2 I1 . . 5_555 177.3(4) ?
I1 Pb2 I2 . . . 90.5(3) ?
I1 Pb2 I2 . . 5_455 90.0(3) ?
I1 Pb2 I4 . . . 86.5(4) ?
I1 Pb2 I7 . . . 85.3(4) ?
I1 Pb2 I2 5_555 . . 89.9(3) ?
I1 Pb2 I2 5_555 . 5_455 89.5(3) ?
I1 Pb2 I4 5_555 . . 90.9(4) ?
I1 Pb2 I7 5_555 . . 97.4(4) ?
I2 Pb2 I2 . . 5_455 176.8(4) ?
I2 Pb2 I4 . . . 87.0(4) ?
I2 Pb2 I7 . . . 86.3(4) ?
I2 Pb2 I4 5_455 . . 89.9(4) ?
I2 Pb2 I7 5_455 . . 96.8(4) ?
I4 Pb2 I7 . . . 169.3(3) ?
Pb2 I1 Pb2 . . 5_445 177.3(6) ?
Pb2 I1 N4 . . . 90.4(7) ?
Pb2 I1 N4 5_445 . . 91.5(7) ?
Pb2 I2 Pb2 . . 5_545 176.8(6) ?
Pb1 I3 Pb1 . . 5_445 178.9(6) ?
Pb1 I4 Pb2 . . . 174.5(5) ?
Pb1 I4 N4 . . . 97.1(7) ?
Pb2 I4 N4 . . . 88.4(7) ?
Pb1 I5 Pb1 . . 5_455 178.6(5) ?
Pb1 I6 Pb1 . . 2_655 174.1(8) ?
Pb1 I6 N1 . . . 93.0(4) ?
Pb1 I6 N1 2_655 . . 93.0(4) ?
Pb2 I7 N2 . . . 98.1(6) ?

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
? ? ? ? ? ? ? ? ? ? ?


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Hydriodic Acid'
