# Electronic Supplementary Material (ESI) for Physical Chemistry Chemical Physics.
# This journal is © the Owner Societies 2023

####################################################################### 
# 
# 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_373K
_database_code_depnum_ccdc_archive 'CCDC 2292085'
loop_
_audit_author_name
_audit_author_address
'Piero Macchi'
;Politecnico di Milano
Italy
;
_audit_update_record             
;
2023-08-31 deposited with the CCDC.	2023-11-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2012
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H8 I3 N4 S10'
_chemical_formula_weight         1005.60

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'

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

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

_cell_length_a                   20.7416(7)
_cell_length_b                   9.9967(3)
_cell_length_c                   7.4017(2)
_cell_angle_alpha                90
_cell_angle_beta                 107.298(3)
_cell_angle_gamma                90
_cell_volume                     1465.31(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    373(2)
_cell_measurement_reflns_used    6035
_cell_measurement_theta_min      2.0390
_cell_measurement_theta_max      26.7890

_exptl_crystal_description       plate
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.261
_exptl_crystal_F_000             950
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.3475
_exptl_crystal_size_mid          0.1364
_exptl_crystal_size_min          0.0264
_exptl_absorpt_coefficient_mu    3.935
_exptl_absorpt_correction_T_min  0.329
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  mirror
_diffrn_ambient_temperature      373(2)
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_detector_area_resol_mean 16.0965
_diffrn_reflns_number            3076
_diffrn_reflns_av_unetI/netI     0.0174
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.057
_diffrn_reflns_theta_max         28.127
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3076
_reflns_number_gt                2451
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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. These statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0616P)²+2.1142P]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3076
_refine_ls_number_parameters     93
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0371
_refine_ls_wR_factor_ref         0.1053
_refine_ls_wR_factor_gt          0.0958
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.044
_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
I1 I 0.5000 0.0000 0.5000 0.0503(2) Uani 1 4 d S T P . .
I2 I 0.35282(3) 0.0000 0.39504(8) 0.0597(2) Uani 1 2 d S T P . .
S1 S 0.61235(9) 0.0000 1.0849(3) 0.0572(5) Uani 1 2 d S T P . .
S2 S 0.92349(6) -0.14788(11) 1.24717(19) 0.0472(3) Uani 1 1 d . . . . .
S3 S 1.08050(7) 0.14648(13) 1.2725(2) 0.0555(3) Uani 1 1 d . . . . .
N1 N 0.6641(2) -0.1255(4) 1.1169(6) 0.0515(10) Uani 1 1 d . . . . .
C1 C 0.7263(2) -0.0713(4) 1.1549(6) 0.0407(9) Uani 1 1 d . . . . .
C2 C 0.7870(2) -0.1436(4) 1.1850(6) 0.0430(10) Uani 1 1 d . . . . .
H2 H 0.7874 -0.2367 1.1873 0.052 Uiso 1 1 calc R U . . .
C3 C 0.8449(2) -0.0720(4) 1.2106(6) 0.0385(9) Uani 1 1 d . . . . .
C4 C 0.9687(3) 0.0000 1.2564(9) 0.0394(13) Uani 1 2 d S T P . .
C5 C 1.0347(3) 0.0000 1.2653(9) 0.0427(14) Uani 1 2 d S T P . .
C6 C 1.1551(3) 0.0659(6) 1.2899(9) 0.0684(16) Uani 1 1 d . . . . .
H6 H 1.1944 0.1138 1.2991 0.082 Uiso 1 1 calc R U . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
I1 0.0493(4) 0.0413(3) 0.0549(4) 0.000 0.0071(3) 0.000
I2 0.0481(3) 0.0626(3) 0.0637(4) 0.000 0.0095(2) 0.000
S1 0.0375(9) 0.0617(11) 0.0716(13) 0.000 0.0147(8) 0.000
S2 0.0387(6) 0.0303(6) 0.0691(8) -0.0017(5) 0.0107(5) 0.0024(4)
S3 0.0473(7) 0.0448(7) 0.0755(9) 0.0044(6) 0.0199(6) -0.0054(6)
N1 0.044(2) 0.049(2) 0.061(3) -0.0014(19) 0.0156(19) -0.0073(18)
C1 0.041(2) 0.036(2) 0.044(2) -0.0035(18) 0.0117(18) -0.0043(18)
C2 0.046(2) 0.029(2) 0.053(3) -0.0008(18) 0.013(2) -0.0021(17)
C3 0.039(2) 0.029(2) 0.043(2) -0.0015(17) 0.0056(17) 0.0006(17)
C4 0.039(3) 0.034(3) 0.043(3) 0.000 0.008(3) 0.000
C5 0.040(3) 0.040(4) 0.047(4) 0.000 0.012(3) 0.000
C6 0.045(3) 0.077(4) 0.090(4) 0.003(3) 0.029(3) -0.007(3)

_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
I1 I2 2.9177(5) . ?
I1 I2 2.9177(5) 5_656 ?
S1 N1 1.622(4) . ?
S1 N1 1.622(4) 6 ?
S2 C4 1.741(4) . ?
S2 C3 1.745(4) . ?
S3 C6 1.715(6) . ?
S3 C5 1.738(4) . ?
N1 C1 1.349(6) . ?
C1 C2 1.411(6) . ?
C1 C1 1.426(8) 6 ?
C2 C3 1.363(6) . ?
C3 C3 1.439(8) 6 ?
C4 C5 1.350(8) . ?
C4 S2 1.741(4) 6 ?
C5 S3 1.738(4) 6 ?
C6 C6 1.317(12) 6 ?

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 I1 I2 180.0 . 5_656 ?
N1 S1 N1 101.3(3) . 6 ?
C4 S2 C3 96.0(2) . . ?
C6 S3 C5 94.6(3) . . ?
C1 N1 S1 105.7(3) . . ?
N1 C1 C2 125.5(4) . . ?
N1 C1 C1 113.7(3) . 6 ?
C2 C1 C1 120.8(2) . 6 ?
C3 C2 C1 117.5(4) . . ?
C2 C3 C3 121.7(3) . 6 ?
C2 C3 S2 122.5(3) . . ?
C3 C3 S2 115.78(14) 6 . ?
C5 C4 S2 121.87(19) . . ?
C5 C4 S2 121.87(19) . 6 ?
S2 C4 S2 116.2(4) . 6 ?
C4 C5 S3 122.60(19) . . ?
C4 C5 S3 122.60(19) . 6 ?
S3 C5 S3 114.8(4) . 6 ?
C6 C6 S3 118.0(2) 6 . ?

_refine_diff_density_max         0.919
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.104

_shelxl_version_number           2012-9

_shelx_res_file                  
;
TITL TTF2I3_373_a_twin1_hklf4 in I2/m
CELL  0.71073  20.7416   9.9967   7.4017   90.000  107.298   90.000
ZERR     2.00   0.0007   0.0003   0.0002    0.000    0.003    0.000
LATT   7
SYMM  - X,   Y, - Z
SFAC  C    H    N    S    I
UNIT  40   0    8    20   6
MERG   2
FMAP   2
PLAN   20
ACTA
L.S.  10
TEMP   100.00
WGHT    0.061600    2.114200
BASF   0.41484
FVAR       2.23929
I1    5    0.500000    0.000000    0.500000    10.25000    0.04927    0.04132 =
         0.05491    0.00000    0.00714    0.00000
I2    5    0.352816    0.000000    0.395042    10.50000    0.04814    0.06263 =
         0.06375    0.00000    0.00948    0.00000
S1    4    0.612346    0.000000    1.084886    10.50000    0.03746    0.06166 =
         0.07163    0.00000    0.01475    0.00000
S2    4    0.923487   -0.147877    1.247168    11.00000    0.03867    0.03028 =
         0.06910   -0.00175    0.01075    0.00237
S3    4    1.080498    0.146481    1.272515    11.00000    0.04728    0.04485 =
         0.07550    0.00436    0.01993   -0.00536
N1    3    0.664099   -0.125509    1.116874    11.00000    0.04428    0.04906 =
         0.06120   -0.00143    0.01564   -0.00731
C1    1    0.726274   -0.071345    1.154927    11.00000    0.04124    0.03630 =
         0.04395   -0.00354    0.01172   -0.00426
C2    1    0.786974   -0.143642    1.185011    11.00000    0.04647    0.02872 =
         0.05261   -0.00076    0.01307   -0.00207
AFIX  43
H2    2    0.787441   -0.236658    1.187288    11.00000   -1.20000
AFIX   0
C3    1    0.844890   -0.071989    1.210605    11.00000    0.03885    0.02896 =
         0.04342   -0.00146    0.00556    0.00065
C4    1    0.968681    0.000000    1.256412    10.50000    0.03890    0.03407 =
         0.04258    0.00000    0.00782    0.00000
C5    1    1.034657    0.000000    1.265343    10.50000    0.03974    0.04021 =
         0.04713    0.00000    0.01158    0.00000
C6    1    1.155102    0.065870    1.289919    11.00000    0.04486    0.07674 =
         0.08969    0.00317    0.02942   -0.00730
AFIX  43
H6    2    1.194385    0.113770    1.299085    11.00000   -1.20000
AFIX   0
HKLF    5

REM  TTF2I3_373_a_twin1_hklf4 in I2/m
REM R1 =  0.0371 for    2451 Fo > 4sig(Fo)  and  0.0519 for all    3076 data
REM     93 parameters refined using      0 restraints

END

WGHT      0.0617      2.1026

REM Highest difference peak  0.919,  deepest hole -0.541,  1-sigma level  0.104
Q1    1   0.6490  0.0000  0.9268  10.50000  0.05    0.92
Q2    1   0.5033  0.0000  1.1573  10.50000  0.05    0.79
Q3    1   0.6427  0.0000  1.2387  10.50000  0.05    0.67
Q4    1   0.3602  0.0000  0.3617  10.50000  0.05    0.53
Q5    1   0.3857  0.0000  0.5407  10.50000  0.05    0.50
Q6    1   0.3392  0.0000  0.2887  10.50000  0.05    0.49
Q7    1   0.3493  0.0679  0.4484  11.00000  0.05    0.47
Q8    1   1.0783  0.1541  1.4008  11.00000  0.05    0.43
Q9    1   0.4794  0.0000  0.3626  10.50000  0.05    0.43
Q10   1   0.6727  0.0000  1.3504  10.50000  0.05    0.40
Q11   1   0.8378  0.0000  1.1804  10.50000  0.05    0.37
Q12   1   0.6900 -0.0865  1.2222  11.00000  0.05    0.35
Q13   1   0.3245  0.0854  0.3030  11.00000  0.05    0.33
Q14   1   0.7776 -0.0954  1.2645  11.00000  0.05    0.32
Q15   1   0.8606  0.0000  1.2413  10.50000  0.05    0.30
Q16   1   0.3678  0.1078  0.2956  11.00000  0.05    0.30
Q17   1   1.1204  0.0000  1.2571  10.50000  0.05    0.30
Q18   1   0.6924 -0.1046  1.0887  11.00000  0.05    0.29
Q19   1   0.9004 -0.1464  1.3752  11.00000  0.05    0.29
Q20   1   0.9875 -0.0641  1.4888  11.00000  0.05    0.28
;
_shelx_res_checksum              9598
####################################################################### 
# 
# 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_323K
_database_code_depnum_ccdc_archive 'CCDC 2292086'
loop_
_audit_author_name
_audit_author_address
'Piero Macchi'
;Politecnico di Milano
Italy
;
_audit_update_record             
;
2023-08-31 deposited with the CCDC.	2023-11-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2012
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H8 I3 N4 S10'
_chemical_formula_weight         1005.60

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'

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

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

_cell_length_a                   20.7153(6)
_cell_length_b                   9.9754(3)
_cell_length_c                   7.3562(2)
_cell_angle_alpha                90
_cell_angle_beta                 107.185(2)
_cell_angle_gamma                90
_cell_volume                     1452.25(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    323(2)
_cell_measurement_reflns_used    7295
_cell_measurement_theta_min      2.0400
_cell_measurement_theta_max      27.6250

_exptl_crystal_description       plate
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.281
_exptl_crystal_F_000             950
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.3468
_exptl_crystal_size_mid          0.1464
_exptl_crystal_size_min          0.0194
_exptl_absorpt_coefficient_mu    3.935
_exptl_absorpt_correction_T_min  0.307
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  mirror
_diffrn_ambient_temperature      323(2)
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_detector_area_resol_mean 16.0965
_diffrn_reflns_number            2979
_diffrn_reflns_av_unetI/netI     0.0132
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.058
_diffrn_reflns_theta_max         28.188
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             2979
_reflns_number_gt                2569
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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. These statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0554P)²+2.4463P]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2979
_refine_ls_number_parameters     93
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0326
_refine_ls_wR_factor_ref         0.0905
_refine_ls_wR_factor_gt          0.0852
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_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
I1 I 0.5000 0.0000 0.5000 0.04161(16) Uani 1 4 d S T P . .
I2 I 0.35277(2) 0.0000 0.39549(6) 0.04911(16) Uani 1 2 d S T P . .
S1 S 0.61226(7) 0.0000 1.0844(3) 0.0465(4) Uani 1 2 d S T P . .
S2 S 0.92371(5) -0.14835(9) 1.24736(16) 0.0393(2) Uani 1 1 d . . . . .
S3 S 1.08070(6) 0.14701(11) 1.27216(18) 0.0459(3) Uani 1 1 d . . . . .
N1 N 0.66373(17) -0.1254(3) 1.1159(5) 0.0423(8) Uani 1 1 d . . . . .
C1 C 0.72596(19) -0.0715(4) 1.1543(6) 0.0342(8) Uani 1 1 d . . . . .
C2 C 0.7868(2) -0.1439(4) 1.1847(6) 0.0355(8) Uani 1 1 d . . . . .
H2 H 0.7872 -0.2371 1.1861 0.043 Uiso 1 1 calc R U . . .
C3 C 0.84491(19) -0.0726(3) 1.2118(5) 0.0318(8) Uani 1 1 d . . . . .
C4 C 0.9685(3) 0.0000 1.2562(8) 0.0330(11) Uani 1 2 d S T P . .
C5 C 1.0354(3) 0.0000 1.2662(8) 0.0354(12) Uani 1 2 d S T P . .
C6 C 1.1558(2) 0.0665(5) 1.2889(8) 0.0570(13) Uani 1 1 d . . . . .
H6 H 1.1950 0.1146 1.2977 0.068 Uiso 1 1 calc R U . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
I1 0.0415(3) 0.0345(3) 0.0445(3) 0.000 0.0061(2) 0.000
I2 0.0403(2) 0.0523(3) 0.0510(3) 0.000 0.00780(18) 0.000
S1 0.0305(7) 0.0515(9) 0.0568(10) 0.000 0.0117(6) 0.000
S2 0.0332(5) 0.0255(5) 0.0562(6) -0.0012(4) 0.0087(5) 0.0026(4)
S3 0.0397(6) 0.0376(6) 0.0617(7) 0.0038(5) 0.0171(5) -0.0048(4)
N1 0.0370(18) 0.0399(19) 0.050(2) 0.0002(15) 0.0131(15) -0.0051(14)
C1 0.0333(18) 0.034(2) 0.0355(19) -0.0013(15) 0.0102(15) -0.0034(15)
C2 0.040(2) 0.0221(17) 0.044(2) -0.0006(15) 0.0123(17) 0.0000(14)
C3 0.035(2) 0.0228(18) 0.0343(18) -0.0002(14) 0.0053(14) 0.0016(14)
C4 0.031(3) 0.031(3) 0.035(3) 0.000 0.007(2) 0.000
C5 0.036(3) 0.035(3) 0.037(3) 0.000 0.013(2) 0.000
C6 0.035(2) 0.062(3) 0.078(3) 0.004(2) 0.023(2) -0.006(2)

_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
I1 I2 2.9167(4) . ?
I1 I2 2.9168(4) 5_656 ?
S1 N1 1.615(4) 6 ?
S1 N1 1.615(4) . ?
S2 C4 1.737(3) . ?
S2 C3 1.747(4) . ?
S3 C6 1.722(5) . ?
S3 C5 1.735(3) . ?
N1 C1 1.347(5) . ?
C1 C2 1.411(5) . ?
C1 C1 1.427(7) 6 ?
C2 C3 1.361(5) . ?
C3 C3 1.448(7) 6 ?
C4 C5 1.366(7) . ?
C4 S2 1.737(3) 6 ?
C5 S3 1.735(3) 6 ?
C6 C6 1.326(10) 6 ?

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 I1 I2 180.0 . 5_656 ?
N1 S1 N1 101.5(2) 6 . ?
C4 S2 C3 95.86(19) . . ?
C6 S3 C5 94.5(2) . . ?
C1 N1 S1 105.8(3) . . ?
N1 C1 C2 125.7(4) . . ?
N1 C1 C1 113.5(2) . 6 ?
C2 C1 C1 120.7(2) . 6 ?
C3 C2 C1 117.8(3) . . ?
C2 C3 C3 121.5(2) . 6 ?
C2 C3 S2 122.9(3) . . ?
C3 C3 S2 115.63(12) 6 . ?
C5 C4 S2 121.60(16) . 6 ?
C5 C4 S2 121.60(16) . . ?
S2 C4 S2 116.8(3) 6 . ?
C4 C5 S3 122.30(17) . . ?
C4 C5 S3 122.30(17) . 6 ?
S3 C5 S3 115.4(3) . 6 ?
C6 C6 S3 117.82(17) 6 . ?

_refine_diff_density_max         0.851
_refine_diff_density_min         -0.876
_refine_diff_density_rms         0.111

_shelxl_version_number           2012-9

_shelx_res_file                  
;
TITL TTF2I3_323_a_twin1_hklf4 in I2/m
CELL  0.71073  20.7153   9.9754   7.3562   90.000  107.185   90.000
ZERR     2.00   0.0006   0.0003   0.0002    0.000    0.002    0.000
LATT   7
SYMM  - X,   Y, - Z
SFAC  C    H    N    S    I
UNIT  40   0    8    20   6
MERG   2
FMAP   2
PLAN   20
ACTA
L.S.  10
TEMP    50.00
WGHT    0.055400    2.446300
BASF   0.42087
FVAR       2.31602
I1    5    0.500000    0.000000    0.500000    10.25000    0.04155    0.03449 =
         0.04453    0.00000    0.00615    0.00000
I2    5    0.352772    0.000000    0.395491    10.50000    0.04031    0.05234 =
         0.05099    0.00000    0.00780    0.00000
S1    4    0.612258    0.000000    1.084354    10.50000    0.03054    0.05148 =
         0.05675    0.00000    0.01172    0.00000
S2    4    0.923710   -0.148346    1.247365    11.00000    0.03317    0.02549 =
         0.05622   -0.00119    0.00871    0.00256
S3    4    1.080702    0.147008    1.272164    11.00000    0.03968    0.03758 =
         0.06174    0.00378    0.01709   -0.00477
N1    3    0.663731   -0.125361    1.115881    11.00000    0.03702    0.03988 =
         0.05028    0.00015    0.01315   -0.00513
C1    1    0.725962   -0.071533    1.154350    11.00000    0.03332    0.03364 =
         0.03550   -0.00130    0.01016   -0.00343
C2    1    0.786791   -0.143860    1.184688    11.00000    0.04042    0.02208 =
         0.04381   -0.00059    0.01231   -0.00005
AFIX  43
H2    2    0.787153   -0.237083    1.186100    11.00000   -1.20000
AFIX   0
C3    1    0.844909   -0.072584    1.211811    11.00000    0.03507    0.02280 =
         0.03434   -0.00019    0.00527    0.00158
C4    1    0.968488    0.000000    1.256246    10.50000    0.03103    0.03126 =
         0.03476    0.00000    0.00679    0.00000
C5    1    1.035373    0.000000    1.266199    10.50000    0.03580    0.03504 =
         0.03679    0.00000    0.01272    0.00000
C6    1    1.155754    0.066464    1.288949    11.00000    0.03531    0.06196 =
         0.07804    0.00401    0.02343   -0.00573
AFIX  43
H6    2    1.195004    0.114609    1.297729    11.00000   -1.20000
AFIX   0
HKLF    5

REM  TTF2I3_323_a_twin1_hklf4 in I2/m
REM R1 =  0.0326 for    2569 Fo > 4sig(Fo)  and  0.0404 for all    2979 data
REM     93 parameters refined using      0 restraints

END

WGHT      0.0549      2.4871

REM Highest difference peak  0.851,  deepest hole -0.876,  1-sigma level  0.111
Q1    1   0.6497  0.0000  1.2718  10.50000  0.05    0.85
Q2    1   0.6457  0.0000  0.9325  10.50000  0.05    0.76
Q3    1   0.4962  0.0000  0.8272  10.50000  0.05    0.67
Q4    1   0.3274  0.0000  0.2679  10.50000  0.05    0.49
Q5    1   0.3606  0.0000  0.3570  10.50000  0.05    0.49
Q6    1   0.3415  0.0591  0.4440  11.00000  0.05    0.47
Q7    1   0.3203  0.0000  0.6029  10.50000  0.05    0.46
Q8    1   0.8397  0.0000  1.1978  10.50000  0.05    0.42
Q9    1   0.4759  0.0000  0.3581  10.50000  0.05    0.36
Q10   1   1.1430  0.0572  1.0943  11.00000  0.05    0.35
Q11   1   0.3821  0.0421  0.2183  11.00000  0.05    0.35
Q12   1   0.5409  0.0000  1.0249  10.50000  0.05    0.32
Q13   1   0.3063  0.0416  0.1440  11.00000  0.05    0.32
Q14   1   1.2146  0.1415  1.4779  11.00000  0.05    0.32
Q15   1   0.3542  0.1415  0.5342  11.00000  0.05    0.31
Q16   1   1.2036  0.0000  1.0815  10.50000  0.05    0.29
Q17   1   0.2664  0.0000  0.1845  10.50000  0.05    0.29
Q18   1   0.7918  0.0000  1.3547  10.50000  0.05    0.28
Q19   1   1.2120  0.0000  1.2571  10.50000  0.05    0.28
Q20   1   0.9293  0.0000  1.0357  10.50000  0.05    0.28
;
_shelx_res_checksum              81885
####################################################################### 
# 
# 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_283K
_database_code_depnum_ccdc_archive 'CCDC 2292087'
loop_
_audit_author_name
_audit_author_address
'Piero Macchi'
;Politecnico di Milano
Italy
;
_audit_update_record             
;
2023-08-31 deposited with the CCDC.	2023-11-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2012
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H8 I3 N4 S10'
_chemical_formula_weight         1005.60

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'

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

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

_cell_length_a                   20.718(4)
_cell_length_b                   9.9600(8)
_cell_length_c                   7.3352(8)
_cell_angle_alpha                90
_cell_angle_beta                 107.070(13)
_cell_angle_gamma                90
_cell_volume                     1447.0(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    283(8)
_cell_measurement_reflns_used    1202
_cell_measurement_theta_min      2.0410
_cell_measurement_theta_max      27.1070

_exptl_crystal_description       plate
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.308
_exptl_crystal_F_000             950
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.2736
_exptl_crystal_size_mid          0.0971
_exptl_crystal_size_min          0.0358
_exptl_absorpt_coefficient_mu    4.012
_exptl_absorpt_correction_T_min  0.76260
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      283(8)
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_detector_area_resol_mean 16.0965
_diffrn_reflns_number            2905
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.057
_diffrn_reflns_theta_max         28.087
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.912
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.912
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             2905
_reflns_number_gt                2189
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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. These statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0384P)²]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2905
_refine_ls_number_parameters     93
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0310
_refine_ls_wR_factor_ref         0.0737
_refine_ls_wR_factor_gt          0.0693
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.000
_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
I1 I 0.5000 0.0000 0.5000 0.03741(16) Uani 1 4 d S T P . .
I2 I 0.35275(2) 0.0000 0.39573(6) 0.04452(15) Uani 1 2 d S T P . .
S1 S 0.61214(7) 0.0000 1.0837(2) 0.0427(4) Uani 1 2 d S T P . .
S2 S 0.92370(5) -0.14850(9) 1.24717(15) 0.0359(2) Uani 1 1 d . . . . .
S3 S 1.08080(6) 0.14725(10) 1.27185(17) 0.0422(3) Uani 1 1 d . . . . .
N1 N 0.66360(16) -0.1257(3) 1.1163(5) 0.0382(8) Uani 1 1 d . . . . .
C1 C 0.72590(18) -0.0719(4) 1.1540(5) 0.0302(8) Uani 1 1 d . . . . .
C2 C 0.78684(19) -0.1440(4) 1.1857(5) 0.0318(9) Uani 1 1 d . . . . .
H2 H 0.7874 -0.2374 1.1889 0.038 Uiso 1 1 calc R U . . .
C3 C 0.84491(18) -0.0723(3) 1.2113(5) 0.0285(8) Uani 1 1 d . . . . .
C4 C 0.9690(3) 0.0000 1.2564(7) 0.0299(12) Uani 1 2 d S T P . .
C5 C 1.0353(3) 0.0000 1.2664(7) 0.0311(12) Uani 1 2 d S T P . .
C10 C 1.1558(2) 0.0662(4) 1.2884(7) 0.0514(12) Uani 1 1 d . . . . .
H10 H 1.1951 0.1144 1.2971 0.062 Uiso 1 1 calc R U . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
I1 0.0379(3) 0.0314(3) 0.0385(3) 0.000 0.0044(2) 0.000
I2 0.0373(2) 0.0482(3) 0.0443(3) 0.000 0.00610(18) 0.000
S1 0.0293(8) 0.0463(9) 0.0515(10) 0.000 0.0103(7) 0.000
S2 0.0306(5) 0.0239(5) 0.0499(6) -0.0014(4) 0.0069(5) 0.0017(4)
S3 0.0369(6) 0.0346(6) 0.0561(7) 0.0041(5) 0.0150(5) -0.0041(5)
N1 0.0313(19) 0.038(2) 0.046(2) -0.0001(16) 0.0118(16) -0.0021(15)
C1 0.031(2) 0.030(2) 0.028(2) -0.0009(16) 0.0065(15) -0.0034(16)
C2 0.036(2) 0.0216(19) 0.036(2) 0.0003(16) 0.0078(17) 0.0001(16)
C3 0.030(2) 0.0255(19) 0.0278(19) 0.0002(15) 0.0046(15) 0.0027(16)
C4 0.029(3) 0.025(3) 0.031(3) 0.000 0.003(2) 0.000
C5 0.034(3) 0.030(3) 0.028(3) 0.000 0.007(2) 0.000
C10 0.033(2) 0.054(3) 0.072(3) 0.003(2) 0.023(2) -0.002(2)

_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
I1 I2 2.9193(7) . ?
I1 I2 2.9194(7) 5_656 ?
S1 N1 1.616(3) 6 ?
S1 N1 1.616(3) . ?
S2 C4 1.742(3) . ?
S2 C3 1.749(4) . ?
S3 C10 1.724(4) . ?
S3 C5 1.738(3) . ?
N1 C1 1.349(5) . ?
C1 C2 1.411(5) . ?
C1 C1 1.433(7) 6 ?
C2 C3 1.364(5) . ?
C3 C3 1.440(7) 6 ?
C4 C5 1.355(7) . ?
C4 S2 1.742(3) 6 ?
C5 S3 1.738(3) 6 ?
C10 C10 1.319(9) 6 ?

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 I1 I2 180.0 . 5_656 ?
N1 S1 N1 101.6(2) 6 . ?
C4 S2 C3 96.06(19) . . ?
C10 S3 C5 94.5(2) . . ?
C1 N1 S1 105.8(3) . . ?
N1 C1 C2 126.0(3) . . ?
N1 C1 C1 113.4(2) . 6 ?
C2 C1 C1 120.6(2) . 6 ?
C3 C2 C1 117.8(3) . . ?
C2 C3 C3 121.6(2) . 6 ?
C2 C3 S2 122.7(3) . . ?
C3 C3 S2 115.72(12) 6 . ?
C5 C4 S2 121.88(16) . . ?
C5 C4 S2 121.88(16) . 6 ?
S2 C4 S2 116.2(3) . 6 ?
C4 C5 S3 122.43(16) . 6 ?
C4 C5 S3 122.43(16) . . ?
S3 C5 S3 115.1(3) 6 . ?
C10 C10 S3 117.92(15) 6 . ?

_refine_diff_density_max         1.173
_refine_diff_density_min         -0.893
_refine_diff_density_rms         0.136

_shelxl_version_number           2012-9

_shelx_res_file                  
;
TITL TTF_amb in C2/m
REM  transformed to space group :
CELL   0.71073 20.7182  9.9600  7.3352   90.000  107.070   90.000
ZERR   2        0.0041  0.0008  0.0008    0.000    0.013    0.000
LATT   7
SYMM  - X,   Y, - Z
SFAC  C    H    N    S    I
UNIT  40   16    8    20   6
MERG   0
FMAP   2
ACTA
PLAN   20
L.S.  10
WGHT    0.038400
BASF   0.16951
FVAR       2.02432
I1    5    0.500000    0.000000    0.500000    10.25000    0.03793    0.03141 =
         0.03854    0.00000    0.00444    0.00000
I2    5    0.352748    0.000000    0.395734    10.50000    0.03725    0.04818 =
         0.04435    0.00000    0.00610    0.00000
S1    4    0.612144    0.000000    1.083686    10.50000    0.02932    0.04627 =
         0.05146    0.00000    0.01030    0.00000
S2    4    0.923700   -0.148498    1.247168    11.00000    0.03063    0.02386 =
         0.04995   -0.00137    0.00691    0.00169
S3    4    1.080804    0.147249    1.271854    11.00000    0.03687    0.03457 =
         0.05612    0.00407    0.01499   -0.00408
N1    3    0.663600   -0.125717    1.116303    11.00000    0.03126    0.03799 =
         0.04571   -0.00014    0.01181   -0.00206
C1    1    0.725904   -0.071937    1.154031    11.00000    0.03055    0.03033 =
         0.02828   -0.00087    0.00648   -0.00343
C2    1    0.786843   -0.144032    1.185679    11.00000    0.03551    0.02163 =
         0.03650    0.00034    0.00783    0.00009
AFIX  43
H2    2    0.787391   -0.237376    1.188944    11.00000   -1.20000
AFIX   0
C3    1    0.844908   -0.072306    1.211321    11.00000    0.02977    0.02550 =
         0.02777    0.00017    0.00455    0.00273
C4    1    0.968970    0.000000    1.256446    10.50000    0.02911    0.02513 =
         0.03146    0.00000    0.00274    0.00000
C5    1    1.035301    0.000000    1.266398    10.50000    0.03438    0.02964 =
         0.02822    0.00000    0.00746    0.00000
C10   1    1.155825    0.066215    1.288434    11.00000    0.03289    0.05408 =
         0.07197    0.00263    0.02278   -0.00237
AFIX  43
H10   2    1.195075    0.114360    1.297106    11.00000   -1.20000
AFIX   0
HKLF    5

REM  TTF_amb in C2/m
REM R1 =  0.0310 for    2189 Fo > 4sig(Fo)  and  0.0484 for all    2905 data
REM     93 parameters refined using      0 restraints

END

WGHT      0.0385      0.0000

REM Highest difference peak  1.173,  deepest hole -0.893,  1-sigma level  0.136
Q1    1   0.3539  0.0000  0.2371  10.50000  0.05    1.17
Q2    1   0.5026  0.0000  0.3419  10.50000  0.05    0.89
Q3    1   0.3380  0.0000  0.6121  10.50000  0.05    0.72
Q4    1   0.3519  0.0000  0.5591  10.50000  0.05    0.67
Q5    1   1.1729  0.0000  1.3414  10.50000  0.05    0.61
Q6    1   0.4563  0.0000  0.5161  10.50000  0.05    0.59
Q7    1   1.2555  0.0000  1.2680  10.50000  0.05    0.57
Q8    1   0.3536  0.0817  0.4527  11.00000  0.05    0.56
Q9    1   0.4835  0.0000  0.7392  10.50000  0.05    0.56
Q10   1   0.7288  0.0000  1.1061  10.50000  0.05    0.52
Q11   1   0.6570 -0.0226  1.2056  11.00000  0.05    0.50
Q12   1   0.3980  0.0000  0.3706  10.50000  0.05    0.49
Q13   1   0.9395 -0.1489  1.0169  11.00000  0.05    0.48
Q14   1   0.5080  0.0000  1.0967  10.50000  0.05    0.48
Q15   1   1.1936  0.0000  1.4833  10.50000  0.05    0.48
Q16   1   0.9185 -0.1443  1.1211  11.00000  0.05    0.47
Q17   1   1.2040  0.0000  1.2393  10.50000  0.05    0.46
Q18   1   0.6402 -0.1710  1.0937  11.00000  0.05    0.46
Q19   1   0.3441  0.1013  0.2781  11.00000  0.05    0.45
Q20   1   0.7297  0.0000  1.3387  10.50000  0.05    0.45
;
_shelx_res_checksum              82985
