# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_I005
_database_code_depnum_ccdc_archive 'CCDC 1910346'
loop_
_audit_author_name
_audit_author_address
'Yuki Tanaka'
;NUS
Singapore
;
_audit_update_record             
;
2021-04-21 deposited with the CCDC.	2021-05-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C1.50 H4.50 I1.50 O0.50 Pb0.50 S0.50'
_chemical_formula_weight         340.53

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'
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

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

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

_cell_length_a                   7.7592(2)
_cell_length_b                   11.1022(3)
_cell_length_c                   14.1866(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1222.09(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6740
_cell_measurement_theta_min      2.99
_cell_measurement_theta_max      30.49

_exptl_crystal_description       Block
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      'Not Measured'
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_density_diffrn    3.702
_exptl_crystal_F_000             1168
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.394
_exptl_crystal_size_mid          0.203
_exptl_crystal_size_min          0.186
_exptl_absorpt_coefficient_mu    21.502
_shelx_estimated_absorpt_T_min   0.2984
_shelx_estimated_absorpt_T_max   0.7461
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.2984
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   'Sadabs, (Sheldrick 2012)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Microfocus Sealed Tube'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11373
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.992
_diffrn_reflns_theta_max         30.518
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             1924
_reflns_number_gt                1774
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_bruker_data_scaling   'SADABS V2012/1 (Bruker AXS Inc.)'
_computing_cell_refinement       'APEX3 v2016.1-0 (Bruker AXS)'
_computing_data_collection       'APEX3 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.32B (Bruker AXS Inc., 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL--2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXT--(Sheldrick 2015)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+1.1715P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     'Dual Space'
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.00211(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1924
_refine_ls_number_parameters     58
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0260
_refine_ls_R_factor_gt           0.0225
_refine_ls_wR_factor_ref         0.0471
_refine_ls_wR_factor_gt          0.0458
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_restrained_S_all      1.155
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 1.06465(2) 0.750000 0.75013(2) 0.00943(7) Uani 1 2 d S T P . .
I1 I 0.81799(3) 0.55687(2) 0.84986(2) 0.01174(7) Uani 1 1 d . . . . .
I2 I 0.82133(4) 0.750000 0.57175(3) 0.01423(9) Uani 1 2 d S T P . .
S1 S 0.26553(16) 0.750000 0.34892(10) 0.0101(2) Uani 1 2 d S T P . .
O1 O 0.3069(5) 0.750000 0.2499(3) 0.0170(9) Uani 1 2 d S T P . .
C1 C 0.4472(7) 0.750000 0.4198(4) 0.0144(11) Uani 1 2 d S T P . .
H1A H 0.417(8) 0.750000 0.487(5) 0.021(17) Uiso 1 2 d S . P . .
H1B H 0.506(6) 0.679(4) 0.404(4) 0.029(14) Uiso 1 1 d . . . . .
C2 C 0.1442(5) 0.6239(4) 0.3830(3) 0.0152(8) Uani 1 1 d . . . . .
H2A H 0.124957 0.626273 0.451287 0.023 Uiso 1 1 calc R U . . .
H2B H 0.206979 0.550284 0.366574 0.023 Uiso 1 1 calc R U . . .
H2C H 0.033006 0.624869 0.350318 0.023 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 I2 3.1572(4) . ?
Pb1 I1 3.2035(3) . ?
Pb1 I1 3.2035(3) 7_575 ?
Pb1 I2 3.2175(4) 6_657 ?
Pb1 I1 3.2363(3) 4_566 ?
Pb1 I1 3.2363(3) 6_657 ?
S1 O1 1.441(4) . ?
S1 C1 1.732(5) . ?
S1 C2 1.755(4) 7_575 ?
S1 C2 1.755(4) . ?
C1 H1A 0.99(7) . ?
C1 H1B 0.94(5) . ?
C1 H1B 0.94(5) 7_575 ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I2 Pb1 I1 89.814(8) . . ?
I2 Pb1 I1 89.814(8) . 7_575 ?
I1 Pb1 I1 84.031(9) . 7_575 ?
I2 Pb1 I2 178.481(11) . 6_657 ?
I1 Pb1 I2 91.315(8) . 6_657 ?
I1 Pb1 I2 91.314(8) 7_575 6_657 ?
I2 Pb1 I1 90.683(8) . 4_566 ?
I1 Pb1 I1 179.282(8) . 4_566 ?
I1 Pb1 I1 96.489(7) 7_575 4_566 ?
I2 Pb1 I1 88.179(7) 6_657 4_566 ?
I2 Pb1 I1 90.683(8) . 6_657 ?
I1 Pb1 I1 96.489(7) . 6_657 ?
I1 Pb1 I1 179.281(8) 7_575 6_657 ?
I2 Pb1 I1 88.179(8) 6_657 6_657 ?
I1 Pb1 I1 82.987(9) 4_566 6_657 ?
Pb1 I1 Pb1 74.089(6) . 6_557 ?
Pb1 I2 Pb1 74.970(8) . 6_557 ?
O1 S1 C1 112.6(3) . . ?
O1 S1 C2 112.86(17) . 7_575 ?
C1 S1 C2 106.05(18) . 7_575 ?
O1 S1 C2 112.86(17) . . ?
C1 S1 C2 106.04(18) . . ?
C2 S1 C2 105.8(3) 7_575 . ?
S1 C1 H1A 112(4) . . ?
S1 C1 H1B 105(3) . . ?
H1A C1 H1B 110(4) . . ?
S1 C1 H1B 105(3) . 7_575 ?
H1A C1 H1B 110(4) . 7_575 ?
H1B C1 H1B 114(6) . 7_575 ?
S1 C2 H2A 109.5 . . ?
S1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
S1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?


_refine_diff_density_max         1.346
_refine_diff_density_min         -0.955
_refine_diff_density_rms         0.233



