# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_hcr_210526_3_auto
_database_code_depnum_ccdc_archive 'CCDC 2110568'
loop_
_audit_author_name
_audit_author_address
'Zhong-Xia Wang'
;Nanchang University
China
;
_audit_update_record             
;
2021-09-18 deposited with the CCDC.	2022-01-10 downloaded from the CCDC.
;
_audit_creation_date             2021-07-06
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        '[SAPD]PbI3'
_chemical_formula_moiety         'I3 Pb, C12 H11 N2 O'
_chemical_formula_sum            'C12 H11 I3 N2 O Pb'
_chemical_formula_weight         787.12
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H N O I Pb'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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      monoclinic
_space_group_IT_number           9
_space_group_name_H-M_alt        Ia
_space_group_name_Hall           'I -2ya'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x+1/2, -y, z'
'x+1/2, y+1/2, z+1/2'
'x+1, -y+1/2, z+1/2'

_cell_length_a                   7.8475(3)
_cell_length_b                   14.3845(6)
_cell_length_c                   16.1929(6)
_cell_angle_alpha                90
_cell_angle_beta                 100.385(4)
_cell_angle_gamma                90
_cell_volume                     1797.95(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4090
_cell_measurement_temperature    297.98(10)
_cell_measurement_theta_max      30.8730
_cell_measurement_theta_min      1.9370
_shelx_estimated_absorpt_T_max   0.868
_shelx_estimated_absorpt_T_min   0.670
_exptl_absorpt_coefficient_mu    14.529
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.25550
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.108a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.908
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.796
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            6055
_diffrn_reflns_point_group_measured_fraction_full 0.897
_diffrn_reflns_point_group_measured_fraction_max 0.653
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.830
_diffrn_reflns_theta_min         1.908
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      297.98(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.796
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -68.00  18.00   0.50    1.00    --    5.05 -19.00  60.00  172
  2  ω    -14.00  27.00   0.50    1.00    --   -5.21 -99.00 150.00   82
  3  ω    -68.00  -3.00   0.50    1.00    --    5.05 -37.00-180.00  130
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0185202000
_diffrn_orient_matrix_UB_12      0.0283827000
_diffrn_orient_matrix_UB_13      -0.0331312000
_diffrn_orient_matrix_UB_21      -0.0044610000
_diffrn_orient_matrix_UB_22      -0.0395594000
_diffrn_orient_matrix_UB_23      -0.0264239000
_diffrn_orient_matrix_UB_31      -0.0898512000
_diffrn_orient_matrix_UB_32      0.0078156000
_diffrn_orient_matrix_UB_33      -0.0137482000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.639
_reflns_Friedel_fraction_full    0.795
_reflns_Friedel_fraction_max     0.510
_reflns_number_gt                3127
_reflns_number_total             3690
_reflns_odcompleteness_completeness 99.95
_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 1.171.41.108a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.614
_refine_diff_density_min         -1.699
_refine_diff_density_rms         0.271
_refine_ls_abs_structure_details 
;
 Flack x determined using 1144 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.022(8)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         3690
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0293
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0346P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0729
_refine_ls_wR_factor_ref         0.0746
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C007(H007), C008(H008), C009(H009), C00A(H00A), C00D(H00D), C00E(H00E),
 C00F(H00F), C00G(H00G), C3(H3), C5(H5)
2.b Idealised tetrahedral OH refined as rotating group:
 O005(H005)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb01 Pb 0.54219(7) 0.50031(4) 0.72922(4) 0.04177(7) Uani 1 1 d . . . . .
I002 I 0.24068(5) 0.41615(5) 0.58789(3) 0.05113(19) Uani 1 1 d . . . . .
I003 I 0.84109(5) 0.58259(5) 0.87209(3) 0.05129(19) Uani 1 1 d . . . . .
I004 I 0.29573(12) 0.67736(3) 0.72315(5) 0.05548(14) Uani 1 1 d . . . . .
O005 O 0.2958(9) 0.3954(5) 0.3717(4) 0.0619(19) Uani 1 1 d . . . . .
H005 H 0.291467 0.444845 0.396376 0.093 Uiso 1 1 calc R U . . .
N006 N 0.3371(10) 0.6647(5) 0.4339(4) 0.0422(19) Uani 1 1 d . . . . .
C007 C 0.4415(15) 0.8142(8) 0.4689(6) 0.062(3) Uani 1 1 d . . . . .
H007 H 0.525498 0.859869 0.469330 0.074 Uiso 1 1 calc R U . . .
C008 C 0.4206(14) 0.4342(8) 0.1369(7) 0.065(3) Uani 1 1 d . . . . .
H008 H 0.444528 0.441717 0.083114 0.078 Uiso 1 1 calc R U . . .
C009 C 0.1742(14) 0.7643(9) 0.5036(7) 0.067(3) Uani 1 1 d . . . . .
H009 H 0.077089 0.775826 0.527498 0.080 Uiso 1 1 calc R U . . .
C00A C 0.2943(15) 0.8318(8) 0.5031(7) 0.068(3) Uani 1 1 d . . . . .
H00A H 0.278360 0.889957 0.525573 0.081 Uiso 1 1 calc R U . . .
N00B N 0.3423(10) 0.5780(5) 0.3938(4) 0.0449(18) Uani 1 1 d . . . . .
C00C C 0.3391(11) 0.4115(6) 0.2956(6) 0.045(2) Uani 1 1 d . . . . .
C00D C 0.3775(15) 0.3478(8) 0.1639(7) 0.068(3) Uani 1 1 d . . . . .
H00D H 0.376269 0.296844 0.128385 0.082 Uiso 1 1 calc R U . . .
C00E C 0.3364(14) 0.3354(7) 0.2422(7) 0.065(3) Uani 1 1 d . . . . .
H00E H 0.307124 0.276712 0.259398 0.078 Uiso 1 1 calc R U . . .
C00F C 0.4609(12) 0.7301(7) 0.4353(6) 0.050(3) Uani 1 1 d . . . . .
H00F H 0.559549 0.717122 0.412969 0.060 Uiso 1 1 calc R U . . .
C00G C 0.3850(11) 0.5811(6) 0.3213(5) 0.043(2) Uani 1 1 d . . . . .
H00G H 0.415419 0.637967 0.300697 0.051 Uiso 1 1 calc R U . . .
C1 C 0.3872(12) 0.4988(6) 0.2705(6) 0.043(2) Uani 1 1 d . . . . .
C3 C 0.4276(15) 0.5074(7) 0.1890(6) 0.057(3) Uani 1 1 d . . . . .
H3 H 0.459768 0.565220 0.171114 0.068 Uiso 1 1 calc R U . . .
C5 C 0.1947(12) 0.6801(8) 0.4695(6) 0.054(3) Uani 1 1 d . . . . .
H5 H 0.113035 0.633437 0.470247 0.064 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb01 I002 3.2170(8) . ?
Pb01 I002 3.2238(8) 2_565 ?
Pb01 I003 3.2530(8) 2_465 ?
Pb01 I003 3.2092(8) . ?
Pb01 I004 3.1888(9) . ?
Pb01 I004 3.2512(9) 2_565 ?
O005 H005 0.8200 . ?
O005 C00C 1.355(11) . ?
N006 N00B 1.410(10) . ?
N006 C00F 1.350(12) . ?
N006 C5 1.364(12) . ?
C007 H007 0.9300 . ?
C007 C00A 1.391(16) . ?
C007 C00F 1.346(15) . ?
C008 H008 0.9300 . ?
C008 C00D 1.380(15) . ?
C008 C3 1.345(14) . ?
C009 H009 0.9300 . ?
C009 C00A 1.355(17) . ?
C009 C5 1.352(16) . ?
C00A H00A 0.9300 . ?
N00B C00G 1.279(11) . ?
C00C C00E 1.393(14) . ?
C00C C1 1.392(12) . ?
C00D H00D 0.9300 . ?
C00D C00E 1.376(16) . ?
C00E H00E 0.9300 . ?
C00F H00F 0.9300 . ?
C00G H00G 0.9300 . ?
C00G C1 1.444(12) . ?
C1 C3 1.417(14) . ?
C3 H3 0.9300 . ?
C5 H5 0.9300 . ?

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
I002 Pb01 I002 91.31(2) . 2_565 ?
I002 Pb01 I003 88.80(2) . 2_465 ?
I002 Pb01 I003 179.61(3) 2_565 2_465 ?
I002 Pb01 I004 93.34(2) . 2_565 ?
I002 Pb01 I004 83.97(2) 2_565 2_565 ?
I003 Pb01 I002 179.22(3) . . ?
I003 Pb01 I002 89.45(2) . 2_565 ?
I003 Pb01 I003 90.44(2) . 2_465 ?
I003 Pb01 I004 86.56(2) . 2_565 ?
I004 Pb01 I002 85.09(2) . . ?
I004 Pb01 I002 92.77(2) . 2_565 ?
I004 Pb01 I003 86.87(2) . 2_465 ?
I004 Pb01 I003 96.39(2) 2_565 2_465 ?
I004 Pb01 I003 95.05(2) . . ?
I004 Pb01 I004 176.36(4) . 2_565 ?
Pb01 I002 Pb01 75.064(17) . 2_465 ?
Pb01 I003 Pb01 74.770(17) . 2_565 ?
Pb01 I004 Pb01 75.067(11) . 2_465 ?
C00C O005 H005 109.5 . . ?
C00F N006 N00B 123.0(8) . . ?
C00F N006 C5 121.4(8) . . ?
C5 N006 N00B 115.6(8) . . ?
C00A C007 H007 120.4 . . ?
C00F C007 H007 120.4 . . ?
C00F C007 C00A 119.2(11) . . ?
C00D C008 H008 120.3 . . ?
C3 C008 H008 120.3 . . ?
C3 C008 C00D 119.5(10) . . ?
C00A C009 H009 119.8 . . ?
C5 C009 H009 119.8 . . ?
C5 C009 C00A 120.3(11) . . ?
C007 C00A H00A 120.0 . . ?
C009 C00A C007 120.0(11) . . ?
C009 C00A H00A 120.0 . . ?
C00G N00B N006 115.2(7) . . ?
O005 C00C C00E 116.8(9) . . ?
O005 C00C C1 123.1(8) . . ?
C1 C00C C00E 120.1(9) . . ?
C008 C00D H00D 119.3 . . ?
C00E C00D C008 121.3(10) . . ?
C00E C00D H00D 119.3 . . ?
C00C C00E H00E 120.3 . . ?
C00D C00E C00C 119.4(10) . . ?
C00D C00E H00E 120.3 . . ?
N006 C00F H00F 120.0 . . ?
C007 C00F N006 120.0(10) . . ?
C007 C00F H00F 120.0 . . ?
N00B C00G H00G 119.1 . . ?
N00B C00G C1 121.7(8) . . ?
C1 C00G H00G 119.1 . . ?
C00C C1 C00G 122.8(9) . . ?
C00C C1 C3 118.0(8) . . ?
C3 C1 C00G 119.1(8) . . ?
C008 C3 C1 121.6(10) . . ?
C008 C3 H3 119.2 . . ?
C1 C3 H3 119.2 . . ?
N006 C5 H5 120.5 . . ?
C009 C5 N006 119.0(10) . . ?
C009 C5 H5 120.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O005 C00C C00E C00D 179.4(9) . . . . ?
O005 C00C C1 C00G -4.0(13) . . . . ?
O005 C00C C1 C3 -179.2(8) . . . . ?
N006 N00B C00G C1 -176.7(7) . . . . ?
C008 C00D C00E C00C -0.3(17) . . . . ?
C00A C007 C00F N006 0.9(15) . . . . ?
C00A C009 C5 N006 -0.7(15) . . . . ?
N00B N006 C00F C007 174.8(8) . . . . ?
N00B N006 C5 C009 -175.1(8) . . . . ?
N00B C00G C1 C00C 1.8(13) . . . . ?
N00B C00G C1 C3 177.0(9) . . . . ?
C00C C1 C3 C008 -0.1(15) . . . . ?
C00D C008 C3 C1 -1.8(17) . . . . ?
C00E C00C C1 C00G 177.1(9) . . . . ?
C00E C00C C1 C3 1.8(13) . . . . ?
C00F N006 N00B C00G -43.8(11) . . . . ?
C00F N006 C5 C009 2.9(13) . . . . ?
C00F C007 C00A C009 1.2(16) . . . . ?
C00G C1 C3 C008 -175.6(10) . . . . ?
C1 C00C C00E C00D -1.6(14) . . . . ?
C3 C008 C00D C00E 2.0(17) . . . . ?
C5 N006 N00B C00G 134.1(8) . . . . ?
C5 N006 C00F C007 -3.0(13) . . . . ?
C5 C009 C00A C007 -1.3(16) . . . . ?

_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 2.448
_oxdiff_exptl_absorpt_empirical_full_min 0.640
####################################################################### 
# 
# 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_hcr_auto
_database_code_depnum_ccdc_archive 'CCDC 2110570'
loop_
_audit_author_name
_audit_author_address
'Zhong-Xia Wang'
;Nanchang University
China
;
_audit_update_record             
;
2021-09-18 deposited with the CCDC.	2022-01-10 downloaded from the CCDC.
;
_audit_creation_date             2021-07-28
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        '[SAPD]I'
_chemical_formula_moiety         'I, C12 H11 N2 O'
_chemical_formula_sum            'C12 H11 I N2 O'
_chemical_formula_weight         326.13
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.5159(2)
_cell_length_b                   7.52770(10)
_cell_length_c                   13.7218(2)
_cell_angle_alpha                90
_cell_angle_beta                 106.358(2)
_cell_angle_gamma                90
_cell_volume                     1240.48(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5928
_cell_measurement_temperature    297.89(10)
_cell_measurement_theta_max      75.6940
_cell_measurement_theta_min      3.3570
_shelx_estimated_absorpt_T_max   0.152
_shelx_estimated_absorpt_T_min   0.131
_exptl_absorpt_coefficient_mu    20.133
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.35235
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.108a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.746
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0290
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7438
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.647
_diffrn_reflns_theta_min         3.681
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      297.89(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     37.00  73.00   0.50    0.20    --  107.00 -61.00  30.00   72
  2  ω     35.00  72.00   0.50    0.20    --  107.00 -61.00 120.00   74
  3  ω     42.00  67.00   0.50    0.20    --  107.00 -61.00 150.00   50
  4  ω     45.00  70.00   0.50    0.20    --  107.00 -61.00 -90.00   50
  5  ω     36.00  61.00   0.50    0.20    --  107.00 -61.00-180.00   50
  6  ω     95.00 166.00   0.50    0.20    --  107.00  61.00-180.00  142
  7  ω     93.00 145.00   0.50    0.20    --  107.00  95.00-131.00  104
  8  ω     34.00 106.00   0.50    0.20    --  107.00 -95.00 118.00  144
  9  ω     45.00  74.00   0.50    0.05    --   45.28 -95.00 118.00   58
 10  ω    -21.00  39.00   0.50    0.05    --   45.28 -95.00 118.00  120
 11  ω    -22.00  33.00   0.50    0.05    --  -45.28  19.00 150.00  110
 12  ω    -21.00  25.00   0.50    0.05    --  -45.28  19.00-120.00   92
 13  ω    -24.00  21.00   0.50    0.05    --  -45.28  19.00-150.00   90
 14  ω    -65.00 -28.00   0.50    0.20    -- -102.00  61.00 -60.00   74
 15  ω    -65.00 -30.00   0.50    0.20    -- -102.00  61.00  30.00   70
 16  ω    -55.00 -28.00   0.50    0.20    -- -102.00  77.00  60.00   54
 17  ω    -67.00 -42.00   0.50    0.20    -- -102.00  61.00  60.00   50
 18  ω   -104.00 -78.00   0.50    0.20    -- -102.00  77.00  60.00   52
 19  ω    -59.00  18.00   0.50    0.05    --  -45.28  95.00-131.00  154
 20  ω    -97.00 -43.00   0.50    0.20    -- -102.00  95.00-131.00  108
 21  ω   -120.00 -82.00   0.50    0.20    -- -102.00 -61.00 150.00   76
 22  ω   -175.00-131.00   0.50    0.20    -- -102.00 -61.00 150.00   88
 23  ω   -154.00-129.00   0.50    0.20    -- -102.00 -95.00 118.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0361266000
_diffrn_orient_matrix_UB_12      0.1896479000
_diffrn_orient_matrix_UB_13      0.0369212000
_diffrn_orient_matrix_UB_21      0.1082647000
_diffrn_orient_matrix_UB_22      -0.0237931000
_diffrn_orient_matrix_UB_23      -0.0312771000
_diffrn_orient_matrix_UB_31      -0.0587131000
_diffrn_orient_matrix_UB_32      0.0727426000
_diffrn_orient_matrix_UB_33      -0.1064824000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2299
_reflns_number_total             2458
_reflns_odcompleteness_completeness 99.62
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.854
_refine_diff_density_min         -0.524
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         2458
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0260
_refine_ls_restrained_S_all      1.070
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0435P)²+0.2299P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0693
_refine_ls_wR_factor_ref         0.0699
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C005(H005), C007(H007), C009(H009), C00A(H00A), C00B(H00B), C00C(H00C),
 C00D(H00D), C00E(H00E), C00F(H00F), C00G(H00G)
2.b Idealised tetrahedral OH refined as rotating group:
 O003(H003)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I001 I 0.83404(2) 0.34680(2) 0.92058(2) 0.04448(9) Uani 1 1 d . . . . .
N002 N 0.78813(19) 0.6239(3) 0.33917(17) 0.0380(5) Uani 1 1 d . . . . .
O003 O 0.7642(2) 0.4538(4) 0.66902(16) 0.0710(7) Uani 1 1 d . . . . .
H003 H 0.774994 0.431283 0.729495 0.106 Uiso 1 1 calc R U . . .
N004 N 0.7050(2) 0.6569(3) 0.38910(18) 0.0413(5) Uani 1 1 d . . . . .
C005 C 0.7302(2) 0.6049(4) 0.4811(2) 0.0381(5) Uani 1 1 d . . . . .
H005 H 0.798126 0.549588 0.510340 0.046 Uiso 1 1 calc R U . . .
C006 C 0.6507(2) 0.6334(4) 0.5403(2) 0.0379(6) Uani 1 1 d . . . . .
C007 C 0.8953(3) 0.6682(4) 0.3803(2) 0.0453(6) Uani 1 1 d . . . . .
H007 H 0.918516 0.717954 0.444895 0.054 Uiso 1 1 calc R U . . .
C008 C 0.6709(2) 0.5536(4) 0.63606(19) 0.0426(6) Uani 1 1 d . . . . .
C009 C 0.7508(2) 0.5552(4) 0.24590(19) 0.0466(6) Uani 1 1 d . . . . .
H009 H 0.675709 0.527686 0.219527 0.056 Uiso 1 1 calc R U . . .
C00A C 0.5953(3) 0.5779(4) 0.6924(2) 0.0473(6) Uani 1 1 d . . . . .
H00A H 0.607773 0.524237 0.755699 0.057 Uiso 1 1 calc R U . . .
C00B C 0.5561(2) 0.7387(5) 0.5038(2) 0.0481(6) Uani 1 1 d . . . . .
H00B H 0.542908 0.793447 0.440761 0.058 Uiso 1 1 calc R U . . .
C00C C 0.5023(3) 0.6811(4) 0.6546(3) 0.0526(7) Uani 1 1 d . . . . .
H00C H 0.452262 0.696830 0.692809 0.063 Uiso 1 1 calc R U . . .
C00D C 0.9704(3) 0.6390(4) 0.3255(3) 0.0560(8) Uani 1 1 d . . . . .
H00D H 1.045203 0.666815 0.353555 0.067 Uiso 1 1 calc R U . . .
C00E C 0.4818(2) 0.7623(5) 0.5604(3) 0.0564(7) Uani 1 1 d . . . . .
H00E H 0.418615 0.831977 0.535607 0.068 Uiso 1 1 calc R U . . .
C00F C 0.8239(3) 0.5254(5) 0.1888(2) 0.0556(7) Uani 1 1 d . . . . .
H00F H 0.798738 0.476761 0.124092 0.067 Uiso 1 1 calc R U . . .
C00G C 0.9347(3) 0.5686(5) 0.2290(3) 0.0573(8) Uani 1 1 d . . . . .
H00G H 0.984903 0.550295 0.191299 0.069 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N002 N004 1.420(3) . ?
N002 C007 1.343(4) . ?
N002 C009 1.337(4) . ?
O003 H003 0.8200 . ?
O003 C008 1.355(4) . ?
N004 C005 1.274(4) . ?
C005 H005 0.9300 . ?
C005 C006 1.466(4) . ?
C006 C008 1.401(4) . ?
C006 C00B 1.396(4) . ?
C007 H007 0.9300 . ?
C007 C00D 1.377(5) . ?
C008 C00A 1.393(4) . ?
C009 H009 0.9300 . ?
C009 C00F 1.380(4) . ?
C00A H00A 0.9300 . ?
C00A C00C 1.374(5) . ?
C00B H00B 0.9300 . ?
C00B C00E 1.381(4) . ?
C00C H00C 0.9300 . ?
C00C C00E 1.387(5) . ?
C00D H00D 0.9300 . ?
C00D C00G 1.379(5) . ?
C00E H00E 0.9300 . ?
C00F H00F 0.9300 . ?
C00F C00G 1.379(5) . ?
C00G H00G 0.9300 . ?

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
C007 N002 N004 122.3(2) . . ?
C009 N002 N004 115.0(2) . . ?
C009 N002 C007 122.5(2) . . ?
C008 O003 H003 109.5 . . ?
C005 N004 N002 114.4(2) . . ?
N004 C005 H005 120.4 . . ?
N004 C005 C006 119.1(3) . . ?
C006 C005 H005 120.4 . . ?
C008 C006 C005 119.0(2) . . ?
C00B C006 C005 121.6(3) . . ?
C00B C006 C008 119.4(3) . . ?
N002 C007 H007 120.5 . . ?
N002 C007 C00D 119.1(3) . . ?
C00D C007 H007 120.5 . . ?
O003 C008 C006 117.5(2) . . ?
O003 C008 C00A 123.0(3) . . ?
C00A C008 C006 119.6(3) . . ?
N002 C009 H009 120.1 . . ?
N002 C009 C00F 119.8(3) . . ?
C00F C009 H009 120.1 . . ?
C008 C00A H00A 120.0 . . ?
C00C C00A C008 120.0(3) . . ?
C00C C00A H00A 120.0 . . ?
C006 C00B H00B 119.7 . . ?
C00E C00B C006 120.6(3) . . ?
C00E C00B H00B 119.7 . . ?
C00A C00C H00C 119.5 . . ?
C00A C00C C00E 121.0(3) . . ?
C00E C00C H00C 119.5 . . ?
C007 C00D H00D 120.0 . . ?
C007 C00D C00G 120.0(3) . . ?
C00G C00D H00D 120.0 . . ?
C00B C00E C00C 119.4(3) . . ?
C00B C00E H00E 120.3 . . ?
C00C C00E H00E 120.3 . . ?
C009 C00F H00F 120.4 . . ?
C00G C00F C009 119.2(3) . . ?
C00G C00F H00F 120.4 . . ?
C00D C00G C00F 119.5(3) . . ?
C00D C00G H00G 120.3 . . ?
C00F C00G H00G 120.3 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N002 N004 C005 C006 179.6(2) . . . . ?
N002 C007 C00D C00G 1.3(5) . . . . ?
N002 C009 C00F C00G -0.5(5) . . . . ?
O003 C008 C00A C00C 179.9(3) . . . . ?
N004 N002 C007 C00D -177.2(3) . . . . ?
N004 N002 C009 C00F 177.1(3) . . . . ?
N004 C005 C006 C008 170.7(3) . . . . ?
N004 C005 C006 C00B -9.7(4) . . . . ?
C005 C006 C008 O003 0.2(4) . . . . ?
C005 C006 C008 C00A -179.2(3) . . . . ?
C005 C006 C00B C00E 179.4(3) . . . . ?
C006 C008 C00A C00C -0.7(4) . . . . ?
C006 C00B C00E C00C 0.4(5) . . . . ?
C007 N002 N004 C005 -49.4(4) . . . . ?
C007 N002 C009 C00F 0.9(4) . . . . ?
C007 C00D C00G C00F -1.0(5) . . . . ?
C008 C006 C00B C00E -1.0(5) . . . . ?
C008 C00A C00C C00E 0.1(5) . . . . ?
C009 N002 N004 C005 134.4(3) . . . . ?
C009 N002 C007 C00D -1.3(4) . . . . ?
C009 C00F C00G C00D 0.6(5) . . . . ?
C00A C00C C00E C00B 0.1(5) . . . . ?
C00B C006 C008 O003 -179.4(3) . . . . ?
C00B C006 C008 C00A 1.2(4) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.731
_oxdiff_exptl_absorpt_empirical_full_min 0.592
####################################################################### 
# 
# 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_hcr_210526_3_173k_auto
_database_code_depnum_ccdc_archive 'CCDC 2110569'
loop_
_audit_author_name
_audit_author_address
'Zhong-Xia Wang'
;Nanchang University
China
;
_audit_update_record             
;
2021-09-18 deposited with the CCDC.	2022-01-10 downloaded from the CCDC.
;
_audit_creation_date             2021-07-06
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        '[SAPD]PbI3'
_chemical_formula_moiety         'I3 Pb, C12 H11 N2 O'
_chemical_formula_sum            'C12 H11 I3 N2 O Pb'
_chemical_formula_weight         787.12
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H N O I Pb'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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      monoclinic
_space_group_IT_number           9
_space_group_name_H-M_alt        Ia
_space_group_name_Hall           'I -2ya'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x+1/2, -y, z'
'x+1/2, y+1/2, z+1/2'
'x+1, -y+1/2, z+1/2'

_cell_length_a                   7.8102(2)
_cell_length_b                   14.2865(4)
_cell_length_c                   16.1155(4)
_cell_angle_alpha                90
_cell_angle_beta                 100.552(2)
_cell_angle_gamma                90
_cell_volume                     1767.77(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4869
_cell_measurement_temperature    172.91(16)
_cell_measurement_theta_max      31.1890
_cell_measurement_theta_min      2.7120
_shelx_estimated_absorpt_T_max   0.757
_shelx_estimated_absorpt_T_min   0.589
_exptl_absorpt_coefficient_mu    14.777
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.13788
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.108a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.957
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.792
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            5477
_diffrn_reflns_point_group_measured_fraction_full 0.906
_diffrn_reflns_point_group_measured_fraction_max 0.667
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.623
_diffrn_reflns_theta_min         1.919
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      172.91(16)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.792
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -57.00   9.00   0.50    1.00    --    5.05 -57.00 120.00  132
  2  ω    -12.00  73.00   0.50    1.00    --    5.05   0.00  90.00  170
  3  ω    -12.00  20.00   0.50    1.00    --   -5.21 -99.00-150.00   64
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0199794000
_diffrn_orient_matrix_UB_12      0.0282451000
_diffrn_orient_matrix_UB_13      -0.0331465000
_diffrn_orient_matrix_UB_21      -0.0031404000
_diffrn_orient_matrix_UB_22      -0.0401004000
_diffrn_orient_matrix_UB_23      -0.0261758000
_diffrn_orient_matrix_UB_31      -0.0901556000
_diffrn_orient_matrix_UB_32      0.0076678000
_diffrn_orient_matrix_UB_33      -0.0148338000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.681
_reflns_Friedel_fraction_full    0.811
_reflns_Friedel_fraction_max     0.542
_reflns_number_gt                3460
_reflns_number_total             3640
_reflns_odcompleteness_completeness 99.95
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.135
_refine_diff_density_min         -2.641
_refine_diff_density_rms         0.278
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.058(10)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         3640
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0323
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0601P)²+0.4110P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0861
_refine_ls_wR_factor_ref         0.0868
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.942(10)
 0.058(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C00F) = Uanis(C1) = Uanis(C4) = Uanis(C3)
Uanis(C3) = Uanis(C4)
Uanis(C5) = Uanis(C006) = Uanis(C00A)
Uanis(N005) = Uanis(N00C)
4.a Aromatic/amide H refined with riding coordinates:
 C006(H006), C007(H007), C008(H008), C00A(H00A), C00B(H00B), C00F(H00F),
 C2(H2), C4(H4), C3(H3), C5(H5)
4.b Idealised tetrahedral OH refined as rotating group:
 O009(H009)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb01 Pb 0.50104(9) 0.50035(4) 0.72298(5) 0.02270(12) Uani 1 1 d . . . . .
I02 I 0.80180(7) 0.58321(7) 0.86653(4) 0.0275(2) Uani 1 1 d . . . . .
I003 I 0.25415(15) 0.67841(4) 0.71705(6) 0.03053(17) Uani 1 1 d . . . . .
I004 I 0.19874(7) 0.41659(7) 0.58044(4) 0.0276(2) Uani 1 1 d . . . . .
N005 N 0.2980(13) 0.6659(7) 0.4277(6) 0.0248(14) Uani 1 1 d . . . . .
C006 C 0.4014(17) 0.8154(9) 0.4642(7) 0.0315(15) Uani 1 1 d . . . . .
H006 H 0.488003 0.862492 0.466640 0.038 Uiso 1 1 calc R U . . .
C007 C 0.3865(19) 0.4327(9) 0.1291(8) 0.038(3) Uani 1 1 d . . . . .
H007 H 0.411976 0.439952 0.074057 0.046 Uiso 1 1 calc R U . . .
C008 C 0.2941(15) 0.3326(8) 0.2346(8) 0.031(3) Uani 1 1 d . . . . .
H008 H 0.260315 0.272601 0.251253 0.038 Uiso 1 1 calc R U . . .
O009 O 0.2524(12) 0.3935(6) 0.3647(5) 0.0324(18) Uani 1 1 d . . . . .
H009 H 0.297017 0.434591 0.399321 0.049 Uiso 1 1 calc R U . . .
C00A C 0.4265(16) 0.7314(9) 0.4276(7) 0.0315(15) Uani 1 1 d . . . . .
H00A H 0.526595 0.719136 0.403659 0.038 Uiso 1 1 calc R U . . .
C00B C 0.3392(19) 0.3453(9) 0.1569(9) 0.041(3) Uani 1 1 d . . . . .
H00B H 0.338234 0.292830 0.120644 0.050 Uiso 1 1 calc R U . . .
N00C N 0.3051(12) 0.5781(6) 0.3876(6) 0.0248(14) Uani 1 1 d . . . . .
C00D C 0.2989(14) 0.4096(8) 0.2888(7) 0.027(2) Uani 1 1 d . . . . .
C1 C 0.3530(17) 0.4975(7) 0.2637(8) 0.0287(13) Uani 1 1 d . . . . .
C00F C 0.3521(15) 0.5807(8) 0.3151(7) 0.0287(13) Uani 1 1 d . . . . .
H00F H 0.387151 0.638733 0.294781 0.034 Uiso 1 1 calc R U . . .
C2 C 0.3956(19) 0.5080(8) 0.1829(8) 0.032(3) Uani 1 1 d . . . . .
H2 H 0.430694 0.567371 0.165501 0.038 Uiso 1 1 calc R U . . .
C4 C 0.1578(16) 0.6785(8) 0.4636(7) 0.0287(13) Uani 1 1 d . . . . .
H4 H 0.077586 0.628731 0.464644 0.034 Uiso 1 1 calc R U . . .
C3 C 0.1302(15) 0.7637(9) 0.4990(7) 0.0287(13) Uani 1 1 d . . . . .
H3 H 0.030177 0.774411 0.523490 0.034 Uiso 1 1 calc R U . . .
C5 C 0.2550(17) 0.8341(10) 0.4976(8) 0.0315(15) Uani 1 1 d . . . . .
H5 H 0.238447 0.894367 0.519719 0.038 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb01 I02 3.2429(10) 2_465 ?
Pb01 I02 3.2063(10) . ?
Pb01 I003 3.1830(11) . ?
Pb01 I003 3.2416(11) 2_565 ?
Pb01 I004 3.2088(10) . ?
Pb01 I004 3.2200(10) 2_565 ?
N005 C00A 1.372(16) . ?
N005 N00C 1.417(12) . ?
N005 C4 1.341(15) . ?
C006 H006 0.9500 . ?
C006 C00A 1.366(17) . ?
C006 C5 1.377(17) . ?
C007 H007 0.9500 . ?
C007 C00B 1.398(18) . ?
C007 C2 1.374(17) . ?
C008 H008 0.9500 . ?
C008 C00B 1.373(18) . ?
C008 C00D 1.401(16) . ?
O009 H009 0.8400 . ?
O009 C00D 1.358(14) . ?
C00A H00A 0.9500 . ?
C00B H00B 0.9500 . ?
N00C C00F 1.288(15) . ?
C00D C1 1.409(16) . ?
C1 C00F 1.450(16) . ?
C1 C2 1.409(18) . ?
C00F H00F 0.9500 . ?
C2 H2 0.9500 . ?
C4 H4 0.9500 . ?
C4 C3 1.377(16) . ?
C3 H3 0.9500 . ?
C3 C5 1.403(17) . ?
C5 H5 0.9500 . ?

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
I02 Pb01 I02 90.29(3) . 2_465 ?
I02 Pb01 I003 86.68(3) . 2_565 ?
I02 Pb01 I004 89.71(3) . 2_565 ?
I02 Pb01 I004 179.55(4) . . ?
I003 Pb01 I02 87.04(3) . 2_465 ?
I003 Pb01 I02 94.95(3) . . ?
I003 Pb01 I02 96.08(3) 2_565 2_465 ?
I003 Pb01 I003 176.48(4) . 2_565 ?
I003 Pb01 I004 85.08(3) . . ?
I003 Pb01 I004 92.93(3) . 2_565 ?
I004 Pb01 I02 89.26(3) . 2_465 ?
I004 Pb01 I02 179.97(4) 2_565 2_465 ?
I004 Pb01 I003 83.95(3) 2_565 2_565 ?
I004 Pb01 I003 93.32(3) . 2_565 ?
I004 Pb01 I004 90.73(3) . 2_565 ?
Pb01 I02 Pb01 74.53(2) . 2_565 ?
Pb01 I003 Pb01 74.860(13) . 2_465 ?
Pb01 I004 Pb01 74.81(2) . 2_465 ?
C00A N005 N00C 120.9(10) . . ?
C4 N005 C00A 124.3(10) . . ?
C4 N005 N00C 114.7(9) . . ?
C00A C006 H006 118.9 . . ?
C00A C006 C5 122.3(12) . . ?
C5 C006 H006 118.9 . . ?
C00B C007 H007 120.6 . . ?
C2 C007 H007 120.6 . . ?
C2 C007 C00B 118.8(12) . . ?
C00B C008 H008 120.6 . . ?
C00B C008 C00D 118.8(11) . . ?
C00D C008 H008 120.6 . . ?
C00D O009 H009 109.5 . . ?
N005 C00A H00A 122.1 . . ?
C006 C00A N005 115.8(11) . . ?
C006 C00A H00A 122.1 . . ?
C007 C00B H00B 118.8 . . ?
C008 C00B C007 122.5(11) . . ?
C008 C00B H00B 118.8 . . ?
C00F N00C N005 115.5(9) . . ?
C008 C00D C1 119.8(11) . . ?
O009 C00D C008 116.6(10) . . ?
O009 C00D C1 123.6(11) . . ?
C00D C1 C00F 122.3(12) . . ?
C00D C1 C2 119.6(11) . . ?
C2 C1 C00F 117.9(10) . . ?
N00C C00F C1 121.8(11) . . ?
N00C C00F H00F 119.1 . . ?
C1 C00F H00F 119.1 . . ?
C007 C2 C1 120.4(11) . . ?
C007 C2 H2 119.8 . . ?
C1 C2 H2 119.8 . . ?
N005 C4 H4 120.0 . . ?
N005 C4 C3 119.9(11) . . ?
C3 C4 H4 120.0 . . ?
C4 C3 H3 121.2 . . ?
C4 C3 C5 117.7(12) . . ?
C5 C3 H3 121.2 . . ?
C006 C5 C3 119.8(12) . . ?
C006 C5 H5 120.1 . . ?
C3 C5 H5 120.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N005 N00C C00F C1 -175.3(10) . . . . ?
N005 C4 C3 C5 -1.6(16) . . . . ?
C008 C00D C1 C00F 176.7(11) . . . . ?
C008 C00D C1 C2 2.4(17) . . . . ?
O009 C00D C1 C00F -4.5(18) . . . . ?
O009 C00D C1 C2 -178.8(11) . . . . ?
C00A N005 N00C C00F -42.5(14) . . . . ?
C00A N005 C4 C3 4.2(17) . . . . ?
C00A C006 C5 C3 3.6(18) . . . . ?
C00B C007 C2 C1 -2(2) . . . . ?
C00B C008 C00D O009 179.7(10) . . . . ?
C00B C008 C00D C1 -1.4(17) . . . . ?
N00C N005 C00A C006 176.6(10) . . . . ?
N00C N005 C4 C3 -175.2(9) . . . . ?
C00D C008 C00B C007 -1(2) . . . . ?
C00D C1 C00F N00C 1.5(18) . . . . ?
C00D C1 C2 C007 -0.8(18) . . . . ?
C00F C1 C2 C007 -175.4(13) . . . . ?
C2 C007 C00B C008 3(2) . . . . ?
C2 C1 C00F N00C 176.0(12) . . . . ?
C4 N005 C00A C006 -2.8(16) . . . . ?
C4 N005 N00C C00F 136.9(11) . . . . ?
C4 C3 C5 C006 -2.1(17) . . . . ?
C5 C006 C00A N005 -1.2(17) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.457
_oxdiff_exptl_absorpt_empirical_full_min 0.601
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.942(10)
2 0.058(10)

