# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_TTF2_complex_block
_database_code_depnum_ccdc_archive 'CCDC 1818732'
_audit_update_record             
;
2018-01-23 deposited with the CCDC.
2018-05-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        TTF2_complex_block
_chemical_name_common            TTF2_complex_block
_chemical_melting_point          '>397 K, decomposed'
_chemical_formula_moiety         'C30 H16 F4 I5 S8'
_chemical_formula_sum            'C30 H16 F4 I5 S8'
_chemical_formula_weight         1343.41

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'
F F 0.0171 0.0103 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   12.3537(6)
_cell_length_b                   13.4244(10)
_cell_length_c                   13.8282(10)
_cell_angle_alpha                61.486(7)
_cell_angle_beta                 76.191(5)
_cell_angle_gamma                83.590(5)
_cell_volume                     1956.9(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(1)
_cell_measurement_reflns_used    3444
_cell_measurement_theta_min      3.7950
_cell_measurement_theta_max      27.5480

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.280
_exptl_crystal_F_000             1250
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.14
_exptl_absorpt_coefficient_mu    4.443
_shelx_estimated_absorpt_T_min   0.89440
_shelx_estimated_absorpt_T_max   1.0000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.89440
_exptl_absorpt_correction_T_max  1.00000
_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_absorpt_special_details   ?
_diffrn_ambient_temperature      173(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.0733
_diffrn_reflns_number            14882
_diffrn_reflns_av_unetI/netI     0.0675
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.319
_diffrn_reflns_theta_max         28.594
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.880
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.880
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.880
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             8811
_reflns_number_gt                6022
_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_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    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Ortep 3w'
_computing_publication_material  'Ortep 3w'
_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)+(0.0420P)²+6.9485P] 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         8811
_refine_ls_number_parameters     427
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0855
_refine_ls_R_factor_gt           0.0517
_refine_ls_wR_factor_ref         0.1288
_refine_ls_wR_factor_gt          0.1060
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_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
C1 C 0.5133(5) 0.4772(5) 0.1620(5) 0.0198(13) Uani 1 1 d . . . . .
C2 C 0.4280(5) 0.4663(6) 0.2529(5) 0.0224(14) Uani 1 1 d . . . . .
C3 C 0.6645(5) 0.5615(5) -0.0188(5) 0.0204(13) Uani 1 1 d . . . . .
C4 C 0.6648(5) 0.4483(6) 0.0156(5) 0.0220(14) Uani 1 1 d . . . . .
C5 C 0.2665(5) 0.5088(6) 0.3836(6) 0.0236(14) Uani 1 1 d . . . . .
C6 C 0.2576(5) 0.3978(6) 0.4167(5) 0.0231(14) Uani 1 1 d . . . . .
C7 C 0.7145(5) 0.7863(6) -0.1355(6) 0.0271(15) Uani 1 1 d . . . . .
C8 C 0.6465(6) 0.8637(6) -0.2027(6) 0.0322(17) Uani 1 1 d . . . . .
H8 H 0.617147 0.847412 -0.249619 0.039 Uiso 1 1 calc R U . . .
C9 C 0.6223(7) 0.9646(7) -0.2002(7) 0.042(2) Uani 1 1 d . . . . .
H9 H 0.577676 1.017907 -0.246096 0.051 Uiso 1 1 calc R U . . .
C10 C 0.6647(7) 0.9853(7) -0.1297(8) 0.048(2) Uani 1 1 d . . . . .
C11 C 0.7325(7) 0.9114(8) -0.0607(8) 0.049(2) Uani 1 1 d . . . . .
H11 H 0.758977 0.928374 -0.012679 0.059 Uiso 1 1 calc R U . . .
C12 C 0.7600(6) 0.8112(7) -0.0655(6) 0.0354(18) Uani 1 1 d . . . . .
H12 H 0.808240 0.760334 -0.022563 0.042 Uiso 1 1 calc R U . . .
C13 C 0.7511(5) 0.2439(6) 0.0400(6) 0.0256(15) Uani 1 1 d . . . . .
C14 C 0.6826(6) 0.1655(7) 0.0463(7) 0.0371(18) Uani 1 1 d . . . . .
H14 H 0.633728 0.188181 -0.002233 0.044 Uiso 1 1 calc R U . . .
C15 C 0.6875(7) 0.0519(7) 0.1261(7) 0.041(2) Uani 1 1 d . . . . .
H15 H 0.641246 -0.001925 0.132463 0.050 Uiso 1 1 calc R U . . .
C16 C 0.7609(7) 0.0218(6) 0.1940(7) 0.041(2) Uani 1 1 d . . . . .
C17 C 0.8290(7) 0.0956(7) 0.1911(7) 0.043(2) Uani 1 1 d . . . . .
H17 H 0.876784 0.071343 0.240895 0.051 Uiso 1 1 calc R U . . .
C18 C 0.8258(6) 0.2087(6) 0.1118(6) 0.0341(17) Uani 1 1 d . . . . .
H18 H 0.873351 0.261059 0.106476 0.041 Uiso 1 1 calc R U . . .
C19 C 0.1137(5) 0.6777(6) 0.3257(6) 0.0273(16) Uani 1 1 d . . . . .
C20 C 0.1093(6) 0.7936(7) 0.2899(7) 0.042(2) Uani 1 1 d . . . . .
H20 H 0.145177 0.824313 0.321579 0.051 Uiso 1 1 calc R U . . .
C21 C 0.0517(7) 0.8633(7) 0.2070(8) 0.049(2) Uani 1 1 d . . . . .
H21 H 0.046061 0.940606 0.184573 0.058 Uiso 1 1 calc R U . . .
C22 C 0.0029(7) 0.8169(7) 0.1585(7) 0.042(2) Uani 1 1 d . . . . .
C23 C 0.0062(6) 0.7030(7) 0.1922(7) 0.0365(18) Uani 1 1 d . . . . .
H23 H -0.028000 0.673119 0.158661 0.044 Uiso 1 1 calc R U . . .
C24 C 0.0618(6) 0.6329(6) 0.2776(6) 0.0324(17) Uani 1 1 d . . . . .
H24 H 0.063764 0.555107 0.302352 0.039 Uiso 1 1 calc R U . . .
C25 C 0.1228(5) 0.2267(6) 0.4668(6) 0.0274(16) Uani 1 1 d . . . . .
C26 C 0.0400(6) 0.2608(6) 0.4045(6) 0.0332(17) Uani 1 1 d . . . . .
H26 H -0.000199 0.326316 0.396073 0.040 Uiso 1 1 calc R U . . .
C27 C 0.0157(6) 0.2004(7) 0.3548(6) 0.0358(18) Uani 1 1 d . . . . .
H27 H -0.037355 0.225806 0.310373 0.043 Uiso 1 1 calc R U . . .
C28 C 0.0732(6) 0.1008(7) 0.3734(6) 0.0343(17) Uani 1 1 d . . . . .
C29 C 0.1531(6) 0.0613(7) 0.4379(6) 0.0361(18) Uani 1 1 d . . . . .
H29 H 0.190071 -0.006454 0.449589 0.043 Uiso 1 1 calc R U . . .
C30 C 0.1769(6) 0.1254(6) 0.4847(6) 0.0340(17) Uani 1 1 d . . . . .
H30 H 0.230164 0.099762 0.528929 0.041 Uiso 1 1 calc R U . . .
F1 F 0.6377(5) 1.0846(5) -0.1259(6) 0.0782(18) Uani 1 1 d . . . . .
F2 F 0.7643(5) -0.0882(4) 0.2696(4) 0.0591(14) Uani 1 1 d . . . . .
F3 F -0.0531(5) 0.8844(4) 0.0777(5) 0.0666(16) Uani 1 1 d . . . . .
F4 F 0.0507(4) 0.0388(4) 0.3274(4) 0.0494(12) Uani 1 1 d . . . . .
S1 S 0.56669(13) 0.61023(14) 0.06185(14) 0.0221(3) Uani 1 1 d . . . . .
S2 S 0.57080(13) 0.36602(14) 0.13929(13) 0.0226(3) Uani 1 1 d . . . . .
S3 S 0.38200(13) 0.57962(15) 0.27765(14) 0.0250(4) Uani 1 1 d . . . . .
S4 S 0.36158(13) 0.34032(14) 0.34862(14) 0.0236(4) Uani 1 1 d . . . . .
S5 S 0.75042(14) 0.65704(15) -0.14144(14) 0.0286(4) Uani 1 1 d . . . . .
S6 S 0.74769(14) 0.38820(15) -0.06336(14) 0.0283(4) Uani 1 1 d . . . . .
S7 S 0.17754(16) 0.58732(17) 0.44148(16) 0.0352(4) Uani 1 1 d . . . . .
S8 S 0.15313(15) 0.30909(17) 0.52615(15) 0.0322(4) Uani 1 1 d . . . . .
I1 I 0.33069(4) 0.37674(5) 0.69861(5) 0.04620(16) Uani 1 1 d . . . . .
I2 I 0.48778(4) 0.28641(5) 0.58591(5) 0.04602(16) Uani 1 1 d . . . . .
I3 I 0.000000 0.500000 1.000000 0.0533(3) Uani 1 2 d S . P . .
I4 I 0.16364(5) 0.54016(6) 0.79502(6) 0.0611(2) Uani 1 1 d . . . . .
I5 I 0.500000 0.000000 0.500000 0.0530(2) Uani 1 2 d S . P . .
I6 I 0.65235(5) 0.18793(6) 0.42241(5) 0.0627(2) Uani 1 1 d . . . . .


_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
C1 C2 1.393(9) . ?
C1 S2 1.713(7) . ?
C1 S1 1.734(6) . ?
C2 S4 1.715(7) . ?
C2 S3 1.721(7) . ?
C3 C4 1.359(9) . ?
C3 S1 1.734(6) . ?
C3 S5 1.737(6) . ?
C4 S6 1.736(7) . ?
C4 S2 1.741(6) . ?
C5 C6 1.343(9) . ?
C5 S3 1.750(7) . ?
C5 S7 1.757(7) . ?
C6 S4 1.740(7) . ?
C6 S8 1.750(6) . ?
C7 C8 1.380(10) . ?
C7 C12 1.406(10) . ?
C7 S5 1.778(7) . ?
C8 C9 1.368(11) . ?
C8 H8 0.9300 . ?
C9 C10 1.355(12) . ?
C9 H9 0.9300 . ?
C10 F1 1.359(9) . ?
C10 C11 1.375(12) . ?
C11 C12 1.379(12) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C14 1.381(10) . ?
C13 C18 1.398(9) . ?
C13 S6 1.779(7) . ?
C14 C15 1.398(11) . ?
C14 H14 0.9300 . ?
C15 C16 1.352(11) . ?
C15 H15 0.9300 . ?
C16 F2 1.345(9) . ?
C16 C17 1.351(11) . ?
C17 C18 1.388(10) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C19 C24 1.374(10) . ?
C19 C20 1.388(10) . ?
C19 S7 1.786(8) . ?
C20 C21 1.383(12) . ?
C20 H20 0.9300 . ?
C21 C22 1.370(13) . ?
C21 H21 0.9300 . ?
C22 F3 1.346(9) . ?
C22 C23 1.367(11) . ?
C23 C24 1.390(11) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 C30 1.383(10) . ?
C25 C26 1.392(10) . ?
C25 S8 1.772(8) . ?
C26 C27 1.381(11) . ?
C26 H26 0.9300 . ?
C27 C28 1.380(11) . ?
C27 H27 0.9300 . ?
C28 F4 1.348(9) . ?
C28 C29 1.378(10) . ?
C29 C30 1.388(11) . ?
C29 H29 0.9300 . ?
C30 H30 0.9300 . ?
I1 I2 2.7387(8) . ?
I3 I4 2.9086(8) 2_567 ?
I3 I4 2.9087(8) . ?
I5 I6 2.9274(8) . ?
I5 I6 2.9275(8) 2_656 ?

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
C2 C1 S2 124.3(5) . . ?
C2 C1 S1 119.9(5) . . ?
S2 C1 S1 115.9(3) . . ?
C1 C2 S4 123.0(5) . . ?
C1 C2 S3 122.0(5) . . ?
S4 C2 S3 115.0(4) . . ?
C4 C3 S1 116.8(5) . . ?
C4 C3 S5 123.1(5) . . ?
S1 C3 S5 120.0(4) . . ?
C3 C4 S6 122.4(5) . . ?
C3 C4 S2 116.7(5) . . ?
S6 C4 S2 120.9(4) . . ?
C6 C5 S3 116.5(5) . . ?
C6 C5 S7 126.2(5) . . ?
S3 C5 S7 117.2(4) . . ?
C5 C6 S4 116.4(5) . . ?
C5 C6 S8 124.2(5) . . ?
S4 C6 S8 119.3(4) . . ?
C8 C7 C12 120.3(7) . . ?
C8 C7 S5 120.3(6) . . ?
C12 C7 S5 119.3(6) . . ?
C9 C8 C7 119.8(8) . . ?
C9 C8 H8 120.1 . . ?
C7 C8 H8 120.1 . . ?
C10 C9 C8 118.9(8) . . ?
C10 C9 H9 120.6 . . ?
C8 C9 H9 120.6 . . ?
C9 C10 F1 118.2(9) . . ?
C9 C10 C11 123.9(8) . . ?
F1 C10 C11 117.9(9) . . ?
C10 C11 C12 117.5(8) . . ?
C10 C11 H11 121.2 . . ?
C12 C11 H11 121.2 . . ?
C11 C12 C7 119.6(8) . . ?
C11 C12 H12 120.2 . . ?
C7 C12 H12 120.2 . . ?
C14 C13 C18 119.9(7) . . ?
C14 C13 S6 119.7(5) . . ?
C18 C13 S6 120.3(6) . . ?
C13 C14 C15 119.4(7) . . ?
C13 C14 H14 120.3 . . ?
C15 C14 H14 120.3 . . ?
C16 C15 C14 118.7(7) . . ?
C16 C15 H15 120.7 . . ?
C14 C15 H15 120.7 . . ?
F2 C16 C17 118.7(8) . . ?
F2 C16 C15 117.4(8) . . ?
C17 C16 C15 123.9(7) . . ?
C16 C17 C18 118.2(7) . . ?
C16 C17 H17 120.9 . . ?
C18 C17 H17 120.9 . . ?
C17 C18 C13 119.9(7) . . ?
C17 C18 H18 120.1 . . ?
C13 C18 H18 120.1 . . ?
C24 C19 C20 119.8(7) . . ?
C24 C19 S7 120.7(6) . . ?
C20 C19 S7 119.4(6) . . ?
C21 C20 C19 120.0(8) . . ?
C21 C20 H20 120.0 . . ?
C19 C20 H20 120.0 . . ?
C22 C21 C20 119.1(8) . . ?
C22 C21 H21 120.5 . . ?
C20 C21 H21 120.5 . . ?
F3 C22 C23 118.7(8) . . ?
F3 C22 C21 119.3(8) . . ?
C23 C22 C21 122.0(8) . . ?
C22 C23 C24 118.7(8) . . ?
C22 C23 H23 120.6 . . ?
C24 C23 H23 120.6 . . ?
C19 C24 C23 120.4(7) . . ?
C19 C24 H24 119.8 . . ?
C23 C24 H24 119.8 . . ?
C30 C25 C26 118.4(7) . . ?
C30 C25 S8 121.3(6) . . ?
C26 C25 S8 120.3(6) . . ?
C27 C26 C25 122.0(7) . . ?
C27 C26 H26 119.0 . . ?
C25 C26 H26 119.0 . . ?
C28 C27 C26 117.5(7) . . ?
C28 C27 H27 121.3 . . ?
C26 C27 H27 121.3 . . ?
F4 C28 C29 118.2(7) . . ?
F4 C28 C27 119.1(7) . . ?
C29 C28 C27 122.7(8) . . ?
C28 C29 C30 118.3(7) . . ?
C28 C29 H29 120.8 . . ?
C30 C29 H29 120.8 . . ?
C25 C30 C29 121.1(7) . . ?
C25 C30 H30 119.5 . . ?
C29 C30 H30 119.5 . . ?
C3 S1 C1 95.2(3) . . ?
C1 S2 C4 95.5(3) . . ?
C2 S3 C5 95.3(3) . . ?
C2 S4 C6 95.8(3) . . ?
C3 S5 C7 101.3(3) . . ?
C4 S6 C13 101.5(3) . . ?
C5 S7 C19 100.1(3) . . ?
C6 S8 C25 100.3(3) . . ?
I4 I3 I4 180.0 2_567 . ?
I6 I5 I6 180.0 . 2_656 ?

_refine_diff_density_max         2.884
_refine_diff_density_min         -1.324
_refine_diff_density_rms         0.172

####################################################################### 
# 
# 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_TTF5_Complex
_database_code_depnum_ccdc_archive 'CCDC 1818736'
_audit_update_record             
;
2018-01-23 deposited with the CCDC.
2018-05-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        'TTF5 complex'
_chemical_name_common            'TTF5 complex'
_chemical_melting_point          '>398 K, decomposed'
_chemical_formula_moiety         'C30 H16 F4 I7 S8'
_chemical_formula_sum            'C30 H16 F4 I7 S8'
_chemical_formula_weight         1597.21

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'
F F 0.0171 0.0103 '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           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   24.2826(12)
_cell_length_b                   10.2755(8)
_cell_length_c                   17.1748(10)
_cell_angle_alpha                90
_cell_angle_beta                 96.201(5)
_cell_angle_gamma                90
_cell_volume                     4260.3(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(1)
_cell_measurement_reflns_used    2336
_cell_measurement_theta_min      3.8210
_cell_measurement_theta_max      27.7950

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.490
_exptl_crystal_F_000             2924
_exptl_transmission_factor_min   0.6417
_exptl_transmission_factor_max   1.0000
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_exptl_absorpt_coefficient_mu    5.533
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_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_absorpt_special_details   ?
_diffrn_ambient_temperature      173(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.0733
_diffrn_reflns_number            8049
_diffrn_reflns_av_unetI/netI     0.1059
_diffrn_reflns_av_R_equivalents  0.0643
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.282
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             4159
_reflns_number_gt                2876
_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_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    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Ortep 3w'
_computing_publication_material  'Ortep 3w'
_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)+206.6560P] 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         4159
_refine_ls_number_parameters     231
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.1314
_refine_ls_R_factor_gt           0.0911
_refine_ls_wR_factor_ref         0.1763
_refine_ls_wR_factor_gt          0.1612
_refine_ls_goodness_of_fit_ref   1.181
_refine_ls_restrained_S_all      1.179
_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
C1 C 0.5256(5) 0.5137(13) 0.4837(7) 0.016(3) Uani 1 1 d . U . A 1
C2 C 0.6159(5) 0.6031(14) 0.4501(7) 0.020(3) Uani 1 1 d . . . B 1
C3 C 0.6072(5) 0.4924(15) 0.4058(7) 0.021(3) Uani 1 1 d . . . B 1
C4 C 0.6881(5) 0.7550(14) 0.5411(7) 0.021(3) Uani 1 1 d . U . C 1
C5 C 0.7084(5) 0.6629(16) 0.5961(8) 0.026(3) Uani 1 1 d . U . C 1
H5 H 0.711561 0.575754 0.582683 0.031 Uiso 1 1 calc R U . C 1
C6 C 0.7237(6) 0.7062(18) 0.6713(10) 0.038(4) Uani 1 1 d . . . C 1
C7 C 0.7204(6) 0.8348(17) 0.6935(8) 0.032(4) Uani 1 1 d . U . C 1
H7 H 0.731775 0.860934 0.744517 0.038 Uiso 1 1 calc R U . C 1
C8 C 0.6998(6) 0.9231(18) 0.6377(9) 0.036(4) Uani 1 1 d . . . C 1
H8 H 0.697639 1.010584 0.650979 0.043 Uiso 1 1 calc R U . C 1
C9 C 0.6823(5) 0.8841(15) 0.5626(8) 0.025(3) Uani 1 1 d . U . C 1
H9 H 0.666516 0.944128 0.526223 0.030 Uiso 1 1 calc R U . C 1
C10 C 0.6212(6) 0.2933(16) 0.3082(9) 0.031(4) Uani 1 1 d . . . D 1
C11 C 0.6307(6) 0.1768(18) 0.3482(9) 0.037(4) Uani 1 1 d . . . D 1
H11 H 0.653484 0.176429 0.395265 0.045 Uiso 1 1 calc R U . D 1
C12 C 0.6073(7) 0.0621(18) 0.3202(9) 0.040(4) Uani 1 1 d . . . D 1
H12 H 0.614851 -0.015063 0.347635 0.048 Uiso 0.6 1 calc R U P D 1
C13 C 0.5728(6) 0.0620(17) 0.2518(9) 0.035(4) Uani 1 1 d . . . D 1
H13 H 0.555542 -0.014146 0.232785 0.042 Uiso 1 1 calc R U . D 1
C14 C 0.5640(6) 0.1789(18) 0.2113(9) 0.035(4) Uani 1 1 d . . . D 1
H14 H 0.541775 0.178857 0.163746 0.042 Uiso 0.4 1 calc R U P D 1
C15 C 0.5869(5) 0.2930(16) 0.2388(8) 0.028(4) Uani 1 1 d . . . D 1
H15 H 0.579423 0.369974 0.211165 0.034 Uiso 1 1 calc R U . D 1
F1 F 0.7438(4) 0.6181(12) 0.7245(6) 0.064(3) Uani 1 1 d . . . C 1
F2 F 0.6171(10) -0.045(2) 0.3600(12) 0.040(6) Uani 0.4 1 d . . P E 2
F3 F 0.5268(8) 0.186(2) 0.1498(10) 0.063(5) Uani 0.6 1 d . . P F 3
S1 S 0.56544(14) 0.6429(4) 0.5075(2) 0.0293(9) Uani 1 1 d . . . . .
S2 S 0.54825(14) 0.4090(4) 0.4163(2) 0.0269(9) Uani 1 1 d . . . . .
S3 S 0.67105(15) 0.7088(4) 0.4413(2) 0.0336(10) Uani 1 1 d . . . . .
S4 S 0.65389(16) 0.4385(5) 0.3427(2) 0.0382(11) Uani 1 1 d . . . . .
I1 I 0.70706(5) -0.27935(13) 0.05582(7) 0.0463(3) Uani 1 1 d . . . . .
I2 I 0.60552(7) -0.31960(15) 0.15708(8) 0.0687(5) Uani 1 1 d . . . . .
I3 I 0.500000 -0.3315(2) 0.250000 0.0587(5) Uani 1 2 d S T P . .
I4 I 0.53394(6) -0.09087(18) 0.04226(8) 0.0737(5) Uani 1 1 d . . . . .


_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
C1 C1 1.45(2) 5_666 ?
C1 S1 1.668(13) . ?
C1 S2 1.713(12) . ?
C2 C3 1.37(2) . ?
C2 S1 1.703(12) . ?
C2 S3 1.745(13) . ?
C3 S2 1.695(13) . ?
C3 S4 1.741(13) . ?
C4 C9 1.39(2) . ?
C4 C5 1.39(2) . ?
C4 S3 1.783(13) . ?
C5 C6 1.38(2) . ?
C5 H5 0.9300 . ?
C6 F1 1.339(18) . ?
C6 C7 1.38(2) . ?
C7 C8 1.37(2) . ?
C7 H7 0.9300 . ?
C8 C9 1.373(19) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
C10 C15 1.38(2) . ?
C10 C11 1.39(2) . ?
C10 S4 1.763(17) . ?
C11 C12 1.37(2) . ?
C11 H11 0.9300 . ?
C12 C13 1.37(2) . ?
C12 H12 0.9300 . ?
C13 C14 1.39(2) . ?
C13 H13 0.9300 . ?
C14 C15 1.36(2) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
I1 I1 3.042(2) 7_645 ?
I4 I4 2.792(4) 5_655 ?

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
C1 C1 S1 124.0(13) 5_666 . ?
C1 C1 S2 119.5(13) 5_666 . ?
S1 C1 S2 116.5(6) . . ?
C3 C2 S1 116.4(10) . . ?
C3 C2 S3 122.8(9) . . ?
S1 C2 S3 120.5(9) . . ?
C2 C3 S2 116.1(9) . . ?
C2 C3 S4 122.6(10) . . ?
S2 C3 S4 121.3(9) . . ?
C9 C4 C5 120.6(13) . . ?
C9 C4 S3 119.4(11) . . ?
C5 C4 S3 120.0(11) . . ?
C6 C5 C4 117.2(15) . . ?
C6 C5 H5 121.4 . . ?
C4 C5 H5 121.4 . . ?
F1 C6 C5 117.6(17) . . ?
F1 C6 C7 119.1(16) . . ?
C5 C6 C7 123.3(15) . . ?
C8 C7 C6 117.9(15) . . ?
C8 C7 H7 121.0 . . ?
C6 C7 H7 121.0 . . ?
C9 C8 C7 121.0(16) . . ?
C9 C8 H8 119.5 . . ?
C7 C8 H8 119.5 . . ?
C8 C9 C4 119.9(15) . . ?
C8 C9 H9 120.0 . . ?
C4 C9 H9 120.0 . . ?
C15 C10 C11 118.6(15) . . ?
C15 C10 S4 120.0(13) . . ?
C11 C10 S4 121.4(12) . . ?
C12 C11 C10 121.9(15) . . ?
C12 C11 H11 119.0 . . ?
C10 C11 H11 119.0 . . ?
C13 C12 C11 119.5(17) . . ?
C13 C12 H12 120.3 . . ?
C11 C12 H12 120.3 . . ?
C12 C13 C14 118.4(17) . . ?
C12 C13 H13 120.8 . . ?
C14 C13 H13 120.8 . . ?
C15 C14 C13 122.4(15) . . ?
C15 C14 H14 118.8 . . ?
C13 C14 H14 118.8 . . ?
C14 C15 C10 119.2(16) . . ?
C14 C15 H15 120.4 . . ?
C10 C15 H15 120.4 . . ?
C1 S1 C2 95.7(6) . . ?
C3 S2 C1 95.2(6) . . ?
C2 S3 C4 100.6(6) . . ?
C3 S4 C10 100.3(6) . . ?

_refine_diff_density_max         1.706
_refine_diff_density_min         -2.022
_refine_diff_density_rms         0.227

