# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry A.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_exp_001_twin1_hklf5
_database_code_depnum_ccdc_archive 'CCDC 2299142'
loop_
_audit_author_name
_audit_author_address
'Harry Sansom'
;University of Oxford
United Kingdom
;
_audit_update_record             
;
2023-10-03 deposited with the CCDC.	2024-01-22 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT214_exp_001_twin1_hklf5 
;
PROBLEM: Atom N2        (Anion/Solvent) ADP max/min Ratio        4.7 oblate
RESPONSE: The rotational disorder of the organic molecule is large, and the electron density appears as spherical. The model here uses a carbon atom placed at the centre, with nitrogen bonded to it, with a fixed nitrogen occupancy to make the expected composition. Together, the carbon and nitrogen displacement parameters model the spherical electron density. The rotational disorder cannot be resolved via room temperature XRD. This model is not being used as phase identification, rather than to present a new crystal structure solution and therefore is considered sufficient.
;
_vrf_PLAT260_exp_001_twin1_hklf5 
;
PROBLEM: Large Average Ueq of Residue Including        C1      0.130 Check
RESPONSE: The rotational disorder of the organic molecule is large, and the electron density appears as spherical. The model here uses a carbon atom placed at the centre, with nitrogen bonded to it, with a fixed nitrogen occupancy to make the expected composition. Together, the carbon and nitrogen displacement parameters model the spherical electron density. The rotational disorder cannot be resolved via room temperature XRD. This model is not being used as phase identification, rather than to present a new crystal structure solution and therefore is considered sufficient.
;
# Added during the CSD deposition process: Tuesday 03 October 2023 08:12 PM
# end Validation Reply Form

_audit_creation_date             2023-10-03
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            'formamidinium lead iodide'
_chemical_name_systematic        ?
_chemical_formula_moiety         'I3 Pb, C N2'
_chemical_formula_sum            'C I3 N2 Pb'
_chemical_formula_weight         627.92
_chemical_melting_point          ?
_chemical_oxdiff_formula         'I3 Pb C N2'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      cubic
_space_group_IT_number           221
_space_group_name_H-M_alt        'P m -3 m'
_space_group_name_Hall           '-P 4 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x, -z, y'
'x, -y, -z'
'x, z, -y'
'z, y, -x'
'-x, y, -z'
'-z, y, x'
'z, x, y'
'y, z, x'
'-y, -z, x'
'z, -x, -y'
'-y, z, -x'
'-z, -x, y'
'-z, x, -y'
'y, -z, -x'
'y, x, -z'
'-y, -x, -z'
'-x, z, y'
'-x, -z, -y'
'z, -y, x'
'-z, -y, -x'
'-x, -y, -z'
'y, -x, -z'
'x, y, -z'
'-y, x, -z'
'-x, z, -y'
'-x, y, z'
'-x, -z, y'
'-z, -y, x'
'x, -y, z'
'z, -y, -x'
'-z, -x, -y'
'-y, -z, -x'
'y, z, -x'
'-z, x, y'
'y, -z, x'
'z, x, -y'
'z, -x, y'
'-y, z, x'
'-y, -x, z'
'y, x, z'
'x, -z, -y'
'x, z, y'
'-z, y, -x'
'z, y, x'

_cell_length_a                   6.36382(16)
_cell_length_b                   6.36382(16)
_cell_length_c                   6.36382(16)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     257.724(19)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    1137
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.6050
_cell_measurement_theta_min      4.4940
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    25.275
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.35979
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.94a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    4.046
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             261
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0173
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            274
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.550
_diffrn_reflns_theta_min         3.201
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4015
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -86.00  19.00   1.00    2.98    --  -11.90 -62.00-151.00  105
  2  ω    -20.00  30.00   1.00    2.98    --  -11.90 -99.00  60.00   50
  3  ω   -100.00 -56.00   1.00    2.98    --  -11.90 178.00 -30.00   44
  4  ω   -102.00 -35.00   1.00    2.98    --  -11.90-178.00 150.00   67
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0417633000
_diffrn_orient_matrix_UB_12      0.1031855000
_diffrn_orient_matrix_UB_13      -0.0056403000
_diffrn_orient_matrix_UB_21      -0.0965780000
_diffrn_orient_matrix_UB_22      -0.0411513000
_diffrn_orient_matrix_UB_23      -0.0375474000
_diffrn_orient_matrix_UB_31      -0.0367899000
_diffrn_orient_matrix_UB_32      -0.0091333000
_diffrn_orient_matrix_UB_33      0.1047356000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                262
_reflns_number_total             274
_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         1.295
_refine_diff_density_min         -1.263
_refine_diff_density_rms         0.321
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     9
_refine_ls_number_reflns         274
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0636
_refine_ls_restrained_S_all      1.136
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1305P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1659
_refine_ls_wR_factor_ref         0.1695
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.62(1)
 0.38(1)
2. Others
 Fixed Sof: N2(0.04167)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.000000 0.000000 0.000000 0.0301(10) Uani 1 48 d S T P . .
I1 I 0.000000 0.000000 -0.500000 0.0841(17) Uani 1 16 d S T P . .
C1 C -0.500000 -0.500000 -0.500000 0.11(6) Uani 1 48 d S T P . .
N2 N 0.583(10) 0.583(10) 0.583(10) 0.15(10) Uani 0.25 6 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 I1 3.18191(8) 8_655 ?
Pb1 I1 3.18191(8) 5_545 ?
Pb1 I1 3.18191(8) 5 ?
Pb1 I1 3.18191(8) 1_556 ?
Pb1 I1 3.18191(8) . ?
Pb1 I1 3.18191(8) 8 ?
C1 N2 0.91(11) 27_445 ?
C1 N2 0.91(11) 2_544 ?
C1 N2 0.91(11) 3_554 ?
C1 N2 0.91(11) 28_545 ?
C1 N2 0.91(11) 4_454 ?
C1 N2 0.91(11) 1_444 ?
C1 N2 0.91(11) 26_455 ?
C1 N2 0.91(11) 25 ?
N2 N2 1.05(13) 4_565 ?
N2 N2 1.05(13) 2_655 ?
N2 N2 1.05(13) 27_556 ?
N2 N2 1.49(18) 26_566 ?
N2 N2 1.8(2) 25_666 ?
N2 N2 1.49(18) 28_656 ?
N2 N2 1.49(18) 3_665 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I1 Pb1 I1 90.0 8_655 . ?
I1 Pb1 I1 90.0 . 5_545 ?
I1 Pb1 I1 90.0 8_655 5 ?
I1 Pb1 I1 180.0 5_545 5 ?
I1 Pb1 I1 90.0 1_556 5_545 ?
I1 Pb1 I1 90.0 5_545 8 ?
I1 Pb1 I1 90.0 8_655 5_545 ?
I1 Pb1 I1 90.0 1_556 5 ?
I1 Pb1 I1 180.0 8_655 8 ?
I1 Pb1 I1 90.0 . 8 ?
I1 Pb1 I1 180.0 . 1_556 ?
I1 Pb1 I1 90.0 1_556 8 ?
I1 Pb1 I1 90.0 5 8 ?
I1 Pb1 I1 90.0 . 5 ?
I1 Pb1 I1 90.0 8_655 1_556 ?
Pb1 I1 Pb1 180.0 1_554 . ?
N2 C1 N2 180(7) 25 1_444 ?
N2 C1 N2 70.53(2) 26_455 4_454 ?
N2 C1 N2 70.529(15) 25 26_455 ?
N2 C1 N2 70.53(3) 1_444 4_454 ?
N2 C1 N2 109.47(2) 27_445 4_454 ?
N2 C1 N2 109.47(5) 28_545 3_554 ?
N2 C1 N2 109.471(13) 1_444 26_455 ?
N2 C1 N2 109.471(5) 2_544 27_445 ?
N2 C1 N2 70.529(10) 1_444 2_544 ?
N2 C1 N2 70.529(15) 25 3_554 ?
N2 C1 N2 70.53(4) 26_455 27_445 ?
N2 C1 N2 70.529(13) 25 28_545 ?
N2 C1 N2 109.47(4) 26_455 3_554 ?
N2 C1 N2 109.471(10) 25 27_445 ?
N2 C1 N2 180.00(2) 28_545 4_454 ?
N2 C1 N2 109.47(5) 25 2_544 ?
N2 C1 N2 70.53(5) 1_444 27_445 ?
N2 C1 N2 70.53(3) 28_545 27_445 ?
N2 C1 N2 109.471(5) 2_544 4_454 ?
N2 C1 N2 180.00(2) 2_544 26_455 ?
N2 C1 N2 70.529(13) 3_554 4_454 ?
N2 C1 N2 70.529(8) 2_544 3_554 ?
N2 C1 N2 70.529(8) 28_545 2_544 ?
N2 C1 N2 180(7) 3_554 27_445 ?
N2 C1 N2 109.47(3) 25 4_454 ?
N2 C1 N2 109.47(3) 1_444 3_554 ?
N2 C1 N2 109.471(8) 1_444 28_545 ?
N2 C1 N2 109.471(5) 28_545 26_455 ?
C1 N2 N2 54.736(5) 1_666 4_565 ?
C1 N2 N2 54.736(3) 1_666 2_655 ?
C1 N2 N2 0(7) 1_666 25_666 ?
C1 N2 N2 35.265(5) 1_666 26_566 ?
C1 N2 N2 35.265(10) 1_666 28_656 ?
C1 N2 N2 54.736(5) 1_666 27_556 ?
C1 N2 N2 35.265(15) 1_666 3_665 ?
N2 N2 N2 45.000(5) 4_565 26_566 ?
N2 N2 N2 45.00(3) 4_565 3_665 ?
N2 N2 N2 45.00(2) 2_655 3_665 ?
N2 N2 N2 90.001(15) 2_655 26_566 ?
N2 N2 N2 90.001(8) 27_556 3_665 ?
N2 N2 N2 60.001(8) 3_665 26_566 ?
N2 N2 N2 60.001(13) 28_656 3_665 ?
N2 N2 N2 90.001(8) 4_565 28_656 ?
N2 N2 N2 90.00(3) 4_565 2_655 ?
N2 N2 N2 90.00(2) 27_556 2_655 ?
N2 N2 N2 54.74(2) 27_556 25_666 ?
N2 N2 N2 60.001(3) 28_656 26_566 ?
N2 N2 N2 35.26(3) 26_566 25_666 ?
N2 N2 N2 45.00(2) 27_556 28_656 ?
N2 N2 N2 54.736(18) 4_565 25_666 ?
N2 N2 N2 45.000(10) 27_556 26_566 ?
N2 N2 N2 35.26(2) 28_656 25_666 ?
N2 N2 N2 45.000(8) 2_655 28_656 ?
N2 N2 N2 54.736(15) 2_655 25_666 ?
N2 N2 N2 90.0 4_565 27_556 ?
N2 N2 N2 35.265(18) 3_665 25_666 ?


_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.455
_oxdiff_exptl_absorpt_empirical_full_min 0.530
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_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 0.62(1) 1237 626 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000
1.0000
2 0.38(1) 1241 626 nmt 0.6703 0.6620 -0.3384 -0.6677 0.3351 -0.6660 -0.3275
0.6716 0.6666

_twin_special_details            
;
Component 2 rotated by 70.4098° 
around [0.71 -0.01 -0.71] (reciprocal) or [0.71 -0.01 -0.70] (direct)
;
####################################################################### 
# 
# 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_exp_246
_database_code_depnum_ccdc_archive 'CCDC 2299143'
loop_
_audit_author_name
_audit_author_address
'Harry Sansom'
;University of Oxford
United Kingdom
;
_audit_update_record             
;
2023-10-03 deposited with the CCDC.	2024-01-22 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT260_exp_246             
;
PROBLEM: Large Average Ueq of Residue Including        C1      0.152 Check
RESPONSE: The rotational disorder of the organic molecule is large, and the electron density appears as spherical. The model here uses a carbon atom placed at the centre, with nitrogen bonded to it, with a fixed nitrogen occupancy to make the expected composition. Together, the carbon and nitrogen displacement parameters model the spherical electron density. The rotational disorder cannot be resolved via room temperature XRD. This model is not being used as phase identification, rather than to present a new crystal structure solution and therefore is considered sufficient.
;
# Added during the CSD deposition process: Tuesday 03 October 2023 08:16 PM
# end Validation Reply Form

_audit_creation_date             2023-10-03
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            'formamidinium lead iodide'
_chemical_name_systematic        ?
_chemical_formula_moiety         'I3 Pb, C N2'
_chemical_formula_sum            'C I3 N2 Pb'
_chemical_formula_weight         627.92
_chemical_melting_point          ?
_chemical_oxdiff_formula         'I3 Pb C N2'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      cubic
_space_group_IT_number           221
_space_group_name_H-M_alt        'P m -3 m'
_space_group_name_Hall           '-P 4 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x, -z, y'
'x, -y, -z'
'x, z, -y'
'z, y, -x'
'-x, y, -z'
'-z, y, x'
'z, x, y'
'y, z, x'
'-y, -z, x'
'z, -x, -y'
'-y, z, -x'
'-z, -x, y'
'-z, x, -y'
'y, -z, -x'
'y, x, -z'
'-y, -x, -z'
'-x, z, y'
'-x, -z, -y'
'z, -y, x'
'-z, -y, -x'
'-x, -y, -z'
'y, -x, -z'
'x, y, -z'
'-y, x, -z'
'-x, z, -y'
'-x, y, z'
'-x, -z, y'
'-z, -y, x'
'x, -y, z'
'z, -y, -x'
'-z, -x, -y'
'-y, -z, -x'
'y, z, -x'
'-z, x, y'
'y, -z, x'
'z, x, -y'
'z, -x, y'
'-y, z, x'
'-y, -x, z'
'y, x, z'
'x, -z, -y'
'x, z, y'
'-z, y, -x'
'z, y, x'

_cell_length_a                   6.35293(19)
_cell_length_b                   6.35293(19)
_cell_length_c                   6.35293(19)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     256.40(2)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    202
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.6890
_cell_measurement_theta_min      4.5200
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    25.406
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71019
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    4.067
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             261
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.929
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -3
_diffrn_reflns_number            352
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.929
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.763
_diffrn_reflns_theta_min         4.537
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4015
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     10.00  59.00   1.00    1.00    --   11.66-116.00  32.00   49
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0161733000
_diffrn_orient_matrix_UB_12      -0.0421893000
_diffrn_orient_matrix_UB_13      0.1020828000
_diffrn_orient_matrix_UB_21      0.0551926000
_diffrn_orient_matrix_UB_22      0.0863384000
_diffrn_orient_matrix_UB_23      0.0443515000
_diffrn_orient_matrix_UB_31      -0.0956927000
_diffrn_orient_matrix_UB_32      0.0569110000
_diffrn_orient_matrix_UB_33      0.0084062000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                88
_reflns_number_total             91
_reflns_odcompleteness_completeness 98.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.418
_refine_diff_density_min         -0.651
_refine_diff_density_rms         0.119
_refine_ls_extinction_coef       0.0175(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     9
_refine_ls_number_reflns         91
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0224
_refine_ls_restrained_S_all      1.113
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0106P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0388
_refine_ls_wR_factor_ref         0.0400
_refine_special_details          ?
_olex2_refinement_description    
;
1. Others
 Fixed Sof: N2(0.04167)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.000000 0.000000 0.000000 0.0366(4) Uani 1 48 d S T P . .
I2 I -0.500000 0.000000 0.000000 0.0894(6) Uani 1 16 d S T P . .
C1 C -0.500000 -0.500000 -0.500000 0.17(4) Uani 1 48 d S T P . .
N2 N -0.500000 -0.500000 -0.337(6) 0.131(19) Uani 0.3334 8 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 I2 3.17647(10) 8 ?
Pb1 I2 3.17647(10) 2 ?
Pb1 I2 3.17647(10) 2_565 ?
Pb1 I2 3.17647(10) 1_655 ?
Pb1 I2 3.17647(10) . ?
Pb1 I2 3.17647(10) 8_554 ?
C1 N2 1.04(4) 32_445 ?
C1 N2 1.04(4) . ?
C1 N2 1.04(4) 25_444 ?
C1 N2 1.04(4) 5_545 ?
C1 N2 1.04(4) 29_454 ?
C1 N2 1.04(4) 8_554 ?
N2 N2 1.47(6) 32_445 ?
N2 N2 1.47(6) 5_545 ?
N2 N2 1.47(6) 29_454 ?
N2 N2 1.47(6) 8_554 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I2 Pb1 I2 90.0 8 . ?
I2 Pb1 I2 90.0 . 2 ?
I2 Pb1 I2 90.0 8 2_565 ?
I2 Pb1 I2 180.0 2 2_565 ?
I2 Pb1 I2 90.0 1_655 2 ?
I2 Pb1 I2 90.0 2 8_554 ?
I2 Pb1 I2 90.0 8 1_655 ?
I2 Pb1 I2 90.0 1_655 2_565 ?
I2 Pb1 I2 180.0 8 8_554 ?
I2 Pb1 I2 90.0 . 8_554 ?
I2 Pb1 I2 180.0 . 1_655 ?
I2 Pb1 I2 90.0 1_655 8_554 ?
I2 Pb1 I2 90.0 . 2_565 ?
I2 Pb1 I2 90.0 8 2 ?
I2 Pb1 I2 90.0 2_565 8_554 ?
Pb1 I2 Pb1 180.0 1_455 . ?
N2 C1 N2 90.000(6) 32_445 . ?
N2 C1 N2 90.000(8) 8_554 25_444 ?
N2 C1 N2 90.000(16) 32_445 5_545 ?
N2 C1 N2 90.000(5) 29_454 . ?
N2 C1 N2 90.000(6) 32_445 29_454 ?
N2 C1 N2 90.000(8) 32_445 25_444 ?
N2 C1 N2 90.0 25_444 29_454 ?
N2 C1 N2 90.000(2) 5_545 . ?
N2 C1 N2 90.000(8) 25_444 5_545 ?
N2 C1 N2 90.000(18) 8_554 29_454 ?
N2 C1 N2 90.000(10) 8_554 5_545 ?
N2 C1 N2 180.0 5_545 29_454 ?
N2 C1 N2 180.0 32_445 8_554 ?
N2 C1 N2 90.000(10) 8_554 . ?
N2 C1 N2 180.0 25_444 . ?
C1 N2 N2 45.000(3) . 32_445 ?
C1 N2 N2 45.0 . 29_454 ?
C1 N2 N2 45.000(2) . 5_545 ?
C1 N2 N2 45.000(2) . 8_554 ?
N2 N2 N2 60.000(3) 32_445 29_454 ?
N2 N2 N2 60.000(5) 32_445 5_545 ?
N2 N2 N2 90.0 5_545 29_454 ?
N2 N2 N2 89.999(2) 32_445 8_554 ?
N2 N2 N2 60.000(8) 5_545 8_554 ?
N2 N2 N2 60.000(5) 29_454 8_554 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 C1 N2 N2 180.0 8_554 . . 32_445 ?
N2 C1 N2 N2 -90.0 8_554 . . 5_545 ?
N2 C1 N2 N2 90.0 32_445 . . 5_545 ?
N2 C1 N2 N2 180.000(6) 32_445 . . 8_554 ?
N2 C1 N2 N2 180.0 29_454 . . 5_545 ?
N2 C1 N2 N2 90.000(16) 8_554 . . 29_454 ?
N2 C1 N2 N2 -90.0 5_545 . . 32_445 ?
N2 C1 N2 N2 180.000(14) 5_545 . . 29_454 ?
N2 C1 N2 N2 90.000(10) 5_545 . . 8_554 ?
N2 C1 N2 N2 -90.000(10) 29_454 . . 8_554 ?
N2 C1 N2 N2 90.0 29_454 . . 32_445 ?
N2 C1 N2 N2 -90.000(16) 32_445 . . 29_454 ?


_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.232
_oxdiff_exptl_absorpt_empirical_full_min 0.845
