# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_H-TTF_150K
_database_code_depnum_ccdc_archive 'CCDC 1896674'
loop_
_audit_author_name
_audit_author_address
'Akira Ueda'
;Kumamoto University
Japan
;
_audit_update_record             
;
2019-05-20 deposited with the CCDC.	2019-06-04 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C24 H15 O4 S12'
_chemical_formula_moiety         'C24 H15 O4 S12'
_chemical_formula_weight         752.10
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
_space_group_IT_number           15
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                   29.44(4)
_cell_length_b                   8.383(12)
_cell_length_c                   11.176(17)
_cell_angle_alpha                90.0000
_cell_angle_beta                 101.55(2)
_cell_angle_gamma                90.0000
_cell_volume                     2703(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2941
_cell_measurement_theta_min      3.06
_cell_measurement_theta_max      27.45
_cell_measurement_temperature    150
#------------------------------------------------------------------------------
_exptl_crystal_description       platelet
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.003
_exptl_crystal_density_diffrn    1.848
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1532.00
_exptl_absorpt_coefficient_mu    1.006
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_absorpt_correction_T_min  0.695
_exptl_absorpt_correction_T_max  0.980

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      150
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 7.314
_diffrn_reflns_number            10179
_diffrn_reflns_av_unetI/netI     0.0906
_diffrn_reflns_av_R_equivalents  0.0831
_diffrn_reflns_theta_max         27.556
_diffrn_reflns_theta_min         3.056
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             3075
_reflns_number_gt                1868
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.1010
_refine_ls_R_factor_gt           0.0547
_refine_ls_wR_factor_ref         0.1397
_refine_ls_wR_factor_gt          0.1140
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_number_reflns         3075
_refine_ls_number_parameters     210
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0510P)²+1.2718P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.000
_refine_diff_density_max         0.59
_refine_diff_density_min         -0.51
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.1246 0.1234
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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
S1 S 0.18116(4) -0.01916(14) 0.39658(10) 0.0243(3) Uani 1 1 d . . . . .
S2 S 0.20710(4) 0.21303(14) 0.22157(10) 0.0242(3) Uani 1 1 d . . . . .
S3 S 0.28677(4) -0.01696(14) 0.54534(10) 0.0239(3) Uani 1 1 d . . . . .
S4 S 0.31093(4) 0.22123(14) 0.37359(10) 0.0250(3) Uani 1 1 d . . . . .
S5 S 0.38039(4) -0.04797(15) 0.69106(10) 0.0266(3) Uani 1 1 d . . . . .
S6 S 0.41075(4) 0.23155(15) 0.48436(11) 0.0307(3) Uani 1 1 d . . . . .
O1 O 0.01319(11) 0.0005(4) 0.1516(3) 0.0286(8) Uani 1 1 d . . . . .
O2 O 0.03995(13) 0.2052(4) -0.0159(3) 0.0286(8) Uani 1 1 d . . . . .
C1 C 0.13708(16) 0.0411(5) 0.2783(4) 0.0197(10) Uani 1 1 d . . . . .
C2 C 0.09087(15) -0.0111(6) 0.2636(4) 0.0218(10) Uani 1 1 d . . . . .
C3 C 0.05830(16) 0.0413(5) 0.1673(4) 0.0220(10) Uani 1 1 d . . . . .
C4 C 0.07165(16) 0.1481(5) 0.0801(4) 0.0215(10) Uani 1 1 d . . . . .
C5 C 0.11625(16) 0.2014(5) 0.0945(4) 0.0205(10) Uani 1 1 d . . . . .
C6 C 0.14949(15) 0.1492(5) 0.1943(4) 0.0185(9) Uani 1 1 d . . . . .
C7 C 0.22406(16) 0.0989(6) 0.3525(4) 0.0250(10) Uani 1 1 d . . . . .
C8 C 0.26868(16) 0.1007(5) 0.4176(4) 0.0218(10) Uani 1 1 d . . . . .
C9 C 0.34466(16) 0.0452(5) 0.5671(4) 0.0211(10) Uani 1 1 d . . . . .
C10 C 0.35601(16) 0.1502(6) 0.4879(4) 0.0262(11) Uani 1 1 d . . . . .
C11 C 0.4349(2) 0.0532(12) 0.6946(7) 0.030(2) Uiso 0.86(2) 1 d . . P A 1
C12 C 0.4468(2) 0.0828(8) 0.5690(6) 0.025(2) Uiso 0.86(2) 1 d . . P A 1
C13 C 0.4397(14) -0.002(6) 0.676(4) 0.028(11) Uiso 0.14(2) 1 d . . P A 2
C14 C 0.4439(16) 0.138(6) 0.628(5) 0.053(17) Uiso 0.14(2) 1 d . . P A 2
H1 H 0.000000 0.008(11) 0.250000 0.11(4) Uiso 1 2 d S . P . .
H2 H 0.023(2) 0.151(7) -0.049(6) 0.06(2) Uiso 1 1 d . . . . .
H3 H 0.0836(13) -0.077(4) 0.319(3) 0.003(10) Uiso 1 1 d . . . . .
H4 H 0.1263(14) 0.260(5) 0.049(4) 0.012(12) Uiso 1 1 d . . . . .
H5 H 0.4593(15) -0.016(5) 0.739(4) 0.017(12) Uiso 1 1 d . . . . .
H6 H 0.4362(19) 0.145(7) 0.746(5) 0.056(18) Uiso 1 1 d . . . . .
H7 H 0.4815(18) 0.154(6) 0.583(4) 0.042(15) Uiso 1 1 d . . . . .
H8 H 0.449(2) -0.014(7) 0.534(6) 0.08(2) Uiso 1 1 d . . . . .


#==============================================================================
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       CrystalClear
_computing_data_reduction        CrystalClear
_computing_structure_solution    'SIR2014 (Burla, et al., 2014)'
_computing_structure_refinement  'SHELXL Version 2018/3 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2019)'
_computing_molecular_graphics    'CrystalStructure 4.3'

#==============================================================================
# MOLECULAR GEOMETRY

_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
S1 C1 1.732(5) . ?
S1 C7 1.752(5) . ?
S2 C7 1.736(5) . ?
S2 C6 1.746(5) . ?
S3 C8 1.729(5) . ?
S3 C9 1.752(5) . ?
S4 C8 1.748(5) . ?
S4 C10 1.752(5) . ?
S5 C9 1.748(5) . ?
S5 C11 1.807(7) . ?
S5 C13 1.83(4) . ?
S6 C10 1.758(5) . ?
S6 C12 1.782(6) . ?
S6 C14 1.88(5) . ?
O1 C3 1.349(5) . ?
O1 H1 1.239(6) . ?
O2 C4 1.361(5) . ?
O2 H2 0.71(6) . ?
C1 C6 1.404(6) . ?
C1 C2 1.407(6) . ?
C2 C3 1.363(6) . ?
C2 H3 0.88(4) . ?
C3 C4 1.434(6) . ?
C4 C5 1.366(7) . ?
C5 C6 1.399(6) . ?
C5 H4 0.80(4) . ?
C7 C8 1.368(7) . ?
C9 C10 1.337(6) . ?
C11 C12 1.534(11) . ?
C11 H5 0.98(4) . ?
C11 H6 0.96(6) . ?
C12 H7 1.16(5) . ?
C12 H8 0.91(6) . ?
C13 C14 1.31(7) . ?
C13 H5 0.82(5) . ?
C13 H6 1.47(7) . ?
C14 H6 1.39(8) . ?
C14 H7 1.31(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
C1 S1 C7 95.3(2) . . ?
C7 S2 C6 94.8(2) . . ?
C8 S3 C9 94.3(2) . . ?
C8 S4 C10 94.4(2) . . ?
C9 S5 C11 101.4(3) . . ?
C9 S5 C13 105.6(13) . . ?
C10 S6 C12 99.7(3) . . ?
C10 S6 C14 98.1(15) . . ?
C3 O1 H1 110.3(13) . . ?
C4 O2 H2 119(5) . . ?
C6 C1 C2 119.9(4) . . ?
C6 C1 S1 116.3(3) . . ?
C2 C1 S1 123.9(3) . . ?
C3 C2 C1 120.2(4) . . ?
C3 C2 H3 121(3) . . ?
C1 C2 H3 118(3) . . ?
O1 C3 C2 122.7(4) . . ?
O1 C3 C4 117.8(4) . . ?
C2 C3 C4 119.5(4) . . ?
O2 C4 C5 118.0(4) . . ?
O2 C4 C3 121.1(4) . . ?
C5 C4 C3 120.8(4) . . ?
C4 C5 C6 119.6(4) . . ?
C4 C5 H4 126(3) . . ?
C6 C5 H4 114(3) . . ?
C5 C6 C1 120.0(4) . . ?
C5 C6 S2 122.9(3) . . ?
C1 C6 S2 117.1(3) . . ?
C8 C7 S2 121.7(4) . . ?
C8 C7 S1 121.8(4) . . ?
S2 C7 S1 116.5(3) . . ?
C7 C8 S3 122.5(4) . . ?
C7 C8 S4 121.2(4) . . ?
S3 C8 S4 116.3(3) . . ?
C10 C9 S5 128.9(4) . . ?
C10 C9 S3 118.0(4) . . ?
S5 C9 S3 113.0(3) . . ?
C9 C10 S4 116.9(4) . . ?
C9 C10 S6 128.5(4) . . ?
S4 C10 S6 114.6(3) . . ?
C12 C11 S5 114.9(5) . . ?
C12 C11 H5 106(3) . . ?
S5 C11 H5 107(2) . . ?
C12 C11 H6 115(3) . . ?
S5 C11 H6 109(3) . . ?
H5 C11 H6 103(4) . . ?
C11 C12 S6 112.2(6) . . ?
C11 C12 H7 109(2) . . ?
S6 C12 H7 97(2) . . ?
C11 C12 H8 107(4) . . ?
S6 C12 H8 119(4) . . ?
H7 C12 H8 113(5) . . ?
C14 C13 S5 113(4) . . ?
C14 C13 H5 112(6) . . ?
S5 C13 H5 114(5) . . ?
C14 C13 H6 60(5) . . ?
S5 C13 H6 88(3) . . ?
H5 C13 H6 77(5) . . ?
C13 C14 S6 131(4) . . ?
C13 C14 H6 66(4) . . ?
S6 C14 H6 130(4) . . ?
C13 C14 H7 114(5) . . ?
S6 C14 H7 88(4) . . ?
H6 C14 H7 132(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
C7 S1 C1 C6 1.5(4) . . . . ?
C7 S1 C1 C2 -178.2(4) . . . . ?
C6 C1 C2 C3 0.9(6) . . . . ?
S1 C1 C2 C3 -179.5(3) . . . . ?
C1 C2 C3 O1 -177.1(4) . . . . ?
C1 C2 C3 C4 1.0(7) . . . . ?
O1 C3 C4 O2 -0.6(6) . . . . ?
C2 C3 C4 O2 -178.8(4) . . . . ?
O1 C3 C4 C5 176.2(4) . . . . ?
C2 C3 C4 C5 -2.0(7) . . . . ?
O2 C4 C5 C6 178.0(4) . . . . ?
C3 C4 C5 C6 1.1(7) . . . . ?
C4 C5 C6 C1 0.8(6) . . . . ?
C4 C5 C6 S2 -179.0(3) . . . . ?
C2 C1 C6 C5 -1.8(6) . . . . ?
S1 C1 C6 C5 178.6(3) . . . . ?
C2 C1 C6 S2 178.0(3) . . . . ?
S1 C1 C6 S2 -1.6(4) . . . . ?
C7 S2 C6 C5 -179.4(4) . . . . ?
C7 S2 C6 C1 0.8(4) . . . . ?
C6 S2 C7 C8 180.0(4) . . . . ?
C6 S2 C7 S1 0.2(3) . . . . ?
C1 S1 C7 C8 179.3(4) . . . . ?
C1 S1 C7 S2 -0.9(3) . . . . ?
S2 C7 C8 S3 -177.8(2) . . . . ?
S1 C7 C8 S3 1.9(6) . . . . ?
S2 C7 C8 S4 1.1(6) . . . . ?
S1 C7 C8 S4 -179.1(2) . . . . ?
C9 S3 C8 C7 177.3(4) . . . . ?
C9 S3 C8 S4 -1.7(3) . . . . ?
C10 S4 C8 C7 -176.3(4) . . . . ?
C10 S4 C8 S3 2.7(3) . . . . ?
C11 S5 C9 C10 6.7(6) . . . . ?
C13 S5 C9 C10 -10.2(19) . . . . ?
C11 S5 C9 S3 -175.5(4) . . . . ?
C13 S5 C9 S3 167.6(18) . . . . ?
C8 S3 C9 C10 -0.6(4) . . . . ?
C8 S3 C9 S5 -178.6(2) . . . . ?
S5 C9 C10 S4 -179.7(3) . . . . ?
S3 C9 C10 S4 2.6(5) . . . . ?
S5 C9 C10 S6 -1.2(7) . . . . ?
S3 C9 C10 S6 -178.9(3) . . . . ?
C8 S4 C10 C9 -3.1(4) . . . . ?
C8 S4 C10 S6 178.2(3) . . . . ?
C12 S6 C10 C9 22.1(5) . . . . ?
C14 S6 C10 C9 -4(2) . . . . ?
C12 S6 C10 S4 -159.4(3) . . . . ?
C14 S6 C10 S4 175(2) . . . . ?
C9 S5 C11 C12 -41.2(8) . . . . ?
S5 C11 C12 S6 71.0(8) . . . . ?
C10 S6 C12 C11 -54.8(6) . . . . ?
C9 S5 C13 C14 33(5) . . . . ?
S5 C13 C14 S6 -51(8) . . . . ?
C10 S6 C14 C13 35(7) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O2 H2 O1 . . 5_555 2.602(5) 0.71(6) 1.90(6) 171(8) no

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.



#==============================================================================
#     End of CIF
#==============================================================================
_exptl_crystal_recrystallization_method electrocrystallization
####################################################################### 
# 
# 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_H-TTF_175K
_database_code_depnum_ccdc_archive 'CCDC 1896676'
loop_
_audit_author_name
_audit_author_address
'Akira Ueda'
;Kumamoto University
Japan
;
_audit_update_record             
;
2019-05-20 deposited with the CCDC.	2019-06-04 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C24 H15 O4 S12'
_chemical_formula_moiety         'C24 H15 O4 S12'
_chemical_formula_weight         752.10
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
_space_group_IT_number           15
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                   29.39(2)
_cell_length_b                   8.390(6)
_cell_length_c                   11.172(9)
_cell_angle_alpha                90.0000
_cell_angle_beta                 100.887(13)
_cell_angle_gamma                90.0000
_cell_volume                     2705(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2931
_cell_measurement_theta_min      3.06
_cell_measurement_theta_max      27.47
_cell_measurement_temperature    175
#------------------------------------------------------------------------------
_exptl_crystal_description       platelet
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.003
_exptl_crystal_density_diffrn    1.847
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1532.00
_exptl_absorpt_coefficient_mu    1.005
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_absorpt_correction_T_min  0.766
_exptl_absorpt_correction_T_max  1.000

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      175
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 7.314
_diffrn_reflns_number            6549
_diffrn_reflns_av_unetI/netI     0.0902
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_theta_max         27.503
_diffrn_reflns_theta_min         3.057
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measured_fraction_theta_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             3002
_reflns_number_gt                1871
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.1105
_refine_ls_R_factor_gt           0.0619
_refine_ls_wR_factor_ref         0.1549
_refine_ls_wR_factor_gt          0.1263
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_reflns         3002
_refine_ls_number_parameters     202
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0581P)²+9.6809P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.000
_refine_diff_density_max         0.45
_refine_diff_density_min         -0.48
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.1246 0.1234
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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
S1 S 0.18129(4) -0.01925(15) 0.39674(11) 0.0277(3) Uani 1 1 d . . . . .
S2 S 0.20711(4) 0.21210(16) 0.22185(11) 0.0281(3) Uani 1 1 d . . . . .
S3 S 0.28679(4) -0.01715(16) 0.54533(12) 0.0281(3) Uani 1 1 d . . . . .
S4 S 0.31102(4) 0.22110(16) 0.37399(11) 0.0284(3) Uani 1 1 d . . . . .
S5 S 0.38030(5) -0.04839(17) 0.69067(12) 0.0313(3) Uani 1 1 d . . . . .
S6 S 0.41087(5) 0.23070(18) 0.48413(12) 0.0349(4) Uani 1 1 d . . . . .
O1 O 0.01335(12) 0.0001(4) 0.1519(3) 0.0309(8) Uani 1 1 d . . . . .
O2 O 0.03981(13) 0.2050(4) -0.0153(3) 0.0316(9) Uani 1 1 d . . . . .
C1 C 0.13701(18) 0.0426(5) 0.2774(4) 0.0241(11) Uani 1 1 d . . . . .
C2 C 0.09087(16) -0.0118(6) 0.2642(4) 0.0231(10) Uani 1 1 d . . . . .
H3 H 0.082384 -0.084383 0.321446 0.028 Uiso 1 1 calc R U . . .
C3 C 0.05836(17) 0.0415(6) 0.1675(4) 0.0253(11) Uani 1 1 d . . . . .
C4 C 0.07147(17) 0.1465(6) 0.0801(4) 0.0269(11) Uani 1 1 d . . . . .
C5 C 0.11632(17) 0.2005(6) 0.0941(4) 0.0238(11) Uani 1 1 d . . . . .
H4 H 0.124817 0.272601 0.036572 0.029 Uiso 1 1 calc R U . . .
C6 C 0.14965(17) 0.1485(6) 0.1940(4) 0.0239(11) Uani 1 1 d . . . . .
C7 C 0.22446(18) 0.0981(6) 0.3527(4) 0.0269(11) Uani 1 1 d . . . . .
C8 C 0.26854(17) 0.1004(6) 0.4179(5) 0.0265(11) Uani 1 1 d . . . . .
C9 C 0.34469(17) 0.0449(6) 0.5672(4) 0.0262(11) Uani 1 1 d . . . . .
C10 C 0.35611(16) 0.1517(6) 0.4877(4) 0.0254(11) Uani 1 1 d . . . . .
C11 C 0.4354(3) 0.0512(13) 0.6959(8) 0.033(2) Uiso 0.82(2) 1 d . . P A 1
C12 C 0.4466(2) 0.0831(9) 0.5708(7) 0.030(2) Uiso 0.82(2) 1 d . . P A 1
C13 C 0.4389(12) -0.007(5) 0.669(3) 0.029(10) Uiso 0.18(2) 1 d . . P A 2
C14 C 0.4443(18) 0.150(7) 0.635(5) 0.075(19) Uiso 0.18(2) 1 d . . P A 2
H1 H 0.000000 -0.009(14) 0.250000 0.14(5) Uiso 1 2 d S . P . .
H2 H 0.016(3) 0.134(11) -0.043(8) 0.12(3) Uiso 1 1 d . . . . .
H5 H 0.4588(19) -0.030(6) 0.745(5) 0.045(17) Uiso 1 1 d . . . . .
H6 H 0.435(2) 0.141(8) 0.737(6) 0.07(2) Uiso 1 1 d . . . . .
H7 H 0.474(2) 0.137(8) 0.574(6) 0.058(19) Uiso 1 1 d . . . . .
H8 H 0.442(2) -0.015(8) 0.524(6) 0.07(2) Uiso 1 1 d . . . . .


#==============================================================================
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       CrystalClear
_computing_data_reduction        CrystalClear
_computing_structure_solution    'SIR2014 (Burla, et al., 2014)'
_computing_structure_refinement  'SHELXL Version 2018/3 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2019)'
_computing_molecular_graphics    'CrystalStructure 4.3'

#==============================================================================
# MOLECULAR GEOMETRY

_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
S1 C7 1.748(5) . ?
S1 C1 1.756(5) . ?
S2 C7 1.741(5) . ?
S2 C6 1.742(5) . ?
S3 C8 1.732(5) . ?
S3 C9 1.752(5) . ?
S4 C8 1.748(5) . ?
S4 C10 1.753(5) . ?
S5 C9 1.751(5) . ?
S5 C13 1.82(3) . ?
S5 C11 1.813(8) . ?
S6 C10 1.748(5) . ?
S6 C12 1.786(7) . ?
S6 C14 1.90(5) . ?
O1 C3 1.346(6) . ?
O1 H1 1.235(8) . ?
O2 C4 1.366(6) . ?
O2 H2 0.92(9) . ?
C1 C6 1.387(6) . ?
C1 C2 1.412(7) . ?
C2 C3 1.375(7) . ?
C2 H3 0.9500 . ?
C3 C4 1.421(7) . ?
C4 C5 1.374(7) . ?
C5 C6 1.408(7) . ?
C5 H4 0.9500 . ?
C7 C8 1.361(7) . ?
C9 C10 1.348(7) . ?
C11 C12 1.519(11) . ?
C11 H5 1.05(6) . ?
C11 H6 0.88(7) . ?
C12 H7 0.92(7) . ?
C12 H8 0.96(7) . ?
C13 C14 1.39(7) . ?
C13 H5 0.96(6) . ?
C13 H6 1.47(7) . ?
C14 H6 1.23(8) . ?
C14 H7 1.21(7) . ?

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
C7 S1 C1 95.3(2) . . ?
C7 S2 C6 95.8(2) . . ?
C8 S3 C9 95.0(2) . . ?
C8 S4 C10 94.9(2) . . ?
C9 S5 C13 104.4(11) . . ?
C9 S5 C11 102.5(3) . . ?
C10 S6 C12 100.0(3) . . ?
C10 S6 C14 99.7(16) . . ?
C3 O1 H1 111.8(15) . . ?
C4 O2 H2 113(5) . . ?
C6 C1 C2 120.7(5) . . ?
C6 C1 S1 116.4(4) . . ?
C2 C1 S1 122.9(4) . . ?
C3 C2 C1 119.2(4) . . ?
C3 C2 H3 120.4 . . ?
C1 C2 H3 120.4 . . ?
O1 C3 C2 122.5(4) . . ?
O1 C3 C4 117.2(4) . . ?
C2 C3 C4 120.2(5) . . ?
O2 C4 C5 117.9(4) . . ?
O2 C4 C3 121.7(4) . . ?
C5 C4 C3 120.3(5) . . ?
C4 C5 C6 119.8(4) . . ?
C4 C5 H4 120.1 . . ?
C6 C5 H4 120.1 . . ?
C1 C6 C5 119.8(5) . . ?
C1 C6 S2 116.7(4) . . ?
C5 C6 S2 123.5(4) . . ?
C8 C7 S2 122.7(4) . . ?
C8 C7 S1 121.7(4) . . ?
S2 C7 S1 115.6(3) . . ?
C7 C8 S3 123.2(4) . . ?
C7 C8 S4 121.1(4) . . ?
S3 C8 S4 115.7(3) . . ?
C10 C9 S3 117.5(4) . . ?
C10 C9 S5 129.1(4) . . ?
S3 C9 S5 113.4(3) . . ?
C9 C10 S6 127.8(4) . . ?
C9 C10 S4 116.8(4) . . ?
S6 C10 S4 115.5(3) . . ?
C12 C11 S5 113.5(6) . . ?
C12 C11 H5 111(3) . . ?
S5 C11 H5 102(3) . . ?
C12 C11 H6 111(4) . . ?
S5 C11 H6 108(4) . . ?
H5 C11 H6 110(5) . . ?
C11 C12 S6 114.4(6) . . ?
C11 C12 H7 113(4) . . ?
S6 C12 H7 96(4) . . ?
C11 C12 H8 108(4) . . ?
S6 C12 H8 107(4) . . ?
H7 C12 H8 118(5) . . ?
C14 C13 S5 112(3) . . ?
C14 C13 H5 111(6) . . ?
S5 C13 H5 106(4) . . ?
C14 C13 H6 51(4) . . ?
S5 C13 H6 86(3) . . ?
H5 C13 H6 78(5) . . ?
C13 C14 S6 121(4) . . ?
C13 C14 H6 68(4) . . ?
S6 C14 H6 133(5) . . ?
C13 C14 H7 101(6) . . ?
S6 C14 H7 81(4) . . ?
H6 C14 H7 145(7) . . ?

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
C7 S1 C1 C6 1.9(4) . . . . ?
C7 S1 C1 C2 -178.7(4) . . . . ?
C6 C1 C2 C3 -0.1(7) . . . . ?
S1 C1 C2 C3 -179.5(4) . . . . ?
C1 C2 C3 O1 -177.1(4) . . . . ?
C1 C2 C3 C4 1.8(7) . . . . ?
O1 C3 C4 O2 0.7(7) . . . . ?
C2 C3 C4 O2 -178.3(4) . . . . ?
O1 C3 C4 C5 176.5(4) . . . . ?
C2 C3 C4 C5 -2.5(7) . . . . ?
O2 C4 C5 C6 177.4(4) . . . . ?
C3 C4 C5 C6 1.5(7) . . . . ?
C2 C1 C6 C5 -1.0(7) . . . . ?
S1 C1 C6 C5 178.4(4) . . . . ?
C2 C1 C6 S2 178.1(4) . . . . ?
S1 C1 C6 S2 -2.4(5) . . . . ?
C4 C5 C6 C1 0.3(7) . . . . ?
C4 C5 C6 S2 -178.8(4) . . . . ?
C7 S2 C6 C1 1.6(4) . . . . ?
C7 S2 C6 C5 -179.3(4) . . . . ?
C6 S2 C7 C8 -179.6(4) . . . . ?
C6 S2 C7 S1 -0.3(3) . . . . ?
C1 S1 C7 C8 178.6(4) . . . . ?
C1 S1 C7 S2 -0.8(3) . . . . ?
S2 C7 C8 S3 -177.8(3) . . . . ?
S1 C7 C8 S3 2.9(6) . . . . ?
S2 C7 C8 S4 0.4(6) . . . . ?
S1 C7 C8 S4 -178.9(3) . . . . ?
C9 S3 C8 C7 176.7(4) . . . . ?
C9 S3 C8 S4 -1.6(3) . . . . ?
C10 S4 C8 C7 -176.0(4) . . . . ?
C10 S4 C8 S3 2.3(3) . . . . ?
C8 S3 C9 C10 -0.2(4) . . . . ?
C8 S3 C9 S5 -178.6(3) . . . . ?
C13 S5 C9 C10 -13.1(16) . . . . ?
C11 S5 C9 C10 6.2(6) . . . . ?
C13 S5 C9 S3 165.1(15) . . . . ?
C11 S5 C9 S3 -175.6(4) . . . . ?
S3 C9 C10 S6 -178.2(3) . . . . ?
S5 C9 C10 S6 0.0(7) . . . . ?
S3 C9 C10 S4 1.9(5) . . . . ?
S5 C9 C10 S4 -179.9(3) . . . . ?
C12 S6 C10 C9 20.2(5) . . . . ?
C14 S6 C10 C9 -9(2) . . . . ?
C12 S6 C10 S4 -159.9(3) . . . . ?
C14 S6 C10 S4 171.0(19) . . . . ?
C8 S4 C10 C9 -2.5(4) . . . . ?
C8 S4 C10 S6 177.5(3) . . . . ?
C9 S5 C11 C12 -39.7(8) . . . . ?
S5 C11 C12 S6 69.5(9) . . . . ?
C10 S6 C12 C11 -54.5(7) . . . . ?
C9 S5 C13 C14 43(4) . . . . ?
S5 C13 C14 S6 -64(6) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O2 H2 O1 . . . 2.756(6) 0.92(9) 2.47(9) 98(6) no
O2 H2 O1 . . 5_555 2.614(5) 0.92(9) 1.76(8) 153(9) no

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.


####################################################################### 
# 
# 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_H-TTF_200K
_database_code_depnum_ccdc_archive 'CCDC 1896677'
loop_
_audit_author_name
_audit_author_address
'Akira Ueda'
;Kumamoto University
Japan
;
_audit_update_record             
;
2019-05-20 deposited with the CCDC.	2019-06-04 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C24 H15 O4 S12'
_chemical_formula_moiety         'C24 H15 O4 S12'
_chemical_formula_weight         752.10
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
_space_group_IT_number           15
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                   29.418(15)
_cell_length_b                   8.421(4)
_cell_length_c                   11.195(6)
_cell_angle_alpha                90.0000
_cell_angle_beta                 100.912(7)
_cell_angle_gamma                90.0000
_cell_volume                     2723(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2791
_cell_measurement_theta_min      3.05
_cell_measurement_theta_max      27.48
_cell_measurement_temperature    200
#------------------------------------------------------------------------------
_exptl_crystal_description       platelet
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.003
_exptl_crystal_density_diffrn    1.834
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1532.00
_exptl_absorpt_coefficient_mu    0.998
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_absorpt_correction_T_min  0.817
_exptl_absorpt_correction_T_max  0.997

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      200
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 7.314
_diffrn_reflns_number            10280
_diffrn_reflns_av_unetI/netI     0.0768
_diffrn_reflns_av_R_equivalents  0.0690
_diffrn_reflns_theta_max         27.451
_diffrn_reflns_theta_min         3.048
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             3028
_reflns_number_gt                1903
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.1076
_refine_ls_R_factor_gt           0.0608
_refine_ls_wR_factor_ref         0.1667
_refine_ls_wR_factor_gt          0.1353
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_reflns         3028
_refine_ls_number_parameters     202
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0808P)²+5.3224P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.000
_refine_diff_density_max         0.49
_refine_diff_density_min         -0.46
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.1246 0.1234
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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
S1 S 0.31872(4) -0.01966(15) 0.10351(11) 0.0295(3) Uani 1 1 d . . . . .
S2 S 0.29273(4) 0.21196(15) 0.27736(11) 0.0304(3) Uani 1 1 d . . . . .
S3 S 0.21318(4) -0.01687(15) -0.04532(11) 0.0310(3) Uani 1 1 d . . . . .
S4 S 0.18877(4) 0.22077(15) 0.12576(11) 0.0304(3) Uani 1 1 d . . . . .
S5 S 0.11966(4) -0.04856(16) -0.19032(11) 0.0332(3) Uani 1 1 d . . . . .
S6 S 0.08897(5) 0.22973(17) 0.01601(13) 0.0381(4) Uani 1 1 d . . . . .
O1 O 0.48647(11) -0.0013(4) 0.3480(3) 0.0340(8) Uani 1 1 d . . . . .
O2 O 0.45988(13) 0.2035(4) 0.5142(3) 0.0344(9) Uani 1 1 d . . . . .
C1 C 0.36290(16) 0.0409(5) 0.2225(4) 0.0238(10) Uani 1 1 d . . . . .
C2 C 0.40904(16) -0.0130(5) 0.2352(4) 0.0258(10) Uani 1 1 d . . . . .
H3 H 0.417630 -0.085068 0.178075 0.031 Uiso 1 1 calc R U . . .
C3 C 0.44149(16) 0.0416(6) 0.3327(4) 0.0269(11) Uani 1 1 d . . . . .
C4 C 0.42853(16) 0.1458(5) 0.4190(4) 0.0265(10) Uani 1 1 d . . . . .
C5 C 0.38391(16) 0.2003(5) 0.4050(4) 0.0251(10) Uani 1 1 d . . . . .
H4 H 0.375633 0.273215 0.462001 0.030 Uiso 1 1 calc R U . . .
C6 C 0.35015(16) 0.1478(5) 0.3053(4) 0.0252(10) Uani 1 1 d . . . . .
C7 C 0.27588(17) 0.0975(6) 0.1469(4) 0.0300(11) Uani 1 1 d . . . . .
C8 C 0.23120(16) 0.1004(6) 0.0829(4) 0.0285(11) Uani 1 1 d . . . . .
C9 C 0.15525(16) 0.0439(6) -0.0668(4) 0.0269(11) Uani 1 1 d . . . . .
C10 C 0.14349(17) 0.1508(6) 0.0125(4) 0.0310(11) Uani 1 1 d . . . . .
C11 C 0.0649(3) 0.0498(14) -0.1942(9) 0.038(2) Uiso 0.78(2) 1 d . . P A 1
C12 C 0.0534(2) 0.0817(9) -0.0691(7) 0.032(3) Uiso 0.78(2) 1 d . . P A 1
C13 C 0.0616(10) -0.006(4) -0.168(3) 0.035(8) Uiso 0.22(2) 1 d . . P A 2
C14 C 0.0555(13) 0.156(5) -0.127(4) 0.070(14) Uiso 0.22(2) 1 d . . P A 2
H1 H 0.500000 -0.007(9) 0.250000 0.06(3) Uiso 1 2 d S . P . .
H2 H 0.481(3) 0.140(9) 0.551(7) 0.11(3) Uiso 1 1 d . . . . .
H5 H 0.0412(16) -0.035(5) -0.241(4) 0.023(12) Uiso 1 1 d . . . . .
H6 H 0.067(2) 0.135(8) -0.224(6) 0.054(19) Uiso 1 1 d . . . . .
H7 H 0.023(2) 0.137(7) -0.084(5) 0.050(16) Uiso 1 1 d . . . . .
H8 H 0.053(3) -0.033(9) -0.020(8) 0.12(3) Uiso 1 1 d . . . . .


#==============================================================================
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       CrystalClear
_computing_data_reduction        CrystalClear
_computing_structure_solution    'SIR2014 (Burla, et al., 2014)'
_computing_structure_refinement  'SHELXL Version 2018/3 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2019)'
_computing_molecular_graphics    'CrystalStructure 4.3'

#==============================================================================
# MOLECULAR GEOMETRY

_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
S1 C7 1.741(5) . ?
S1 C1 1.751(5) . ?
S2 C7 1.741(5) . ?
S2 C6 1.744(5) . ?
S3 C8 1.740(5) . ?
S3 C9 1.752(5) . ?
S4 C8 1.744(5) . ?
S4 C10 1.758(5) . ?
S5 C9 1.751(5) . ?
S5 C13 1.81(3) . ?
S5 C11 1.806(8) . ?
S6 C10 1.743(5) . ?
S6 C12 1.783(7) . ?
S6 C14 1.82(4) . ?
O1 C3 1.351(5) . ?
O1 H1 1.237(5) . ?
O2 C4 1.360(5) . ?
O2 H2 0.86(8) . ?
C1 C6 1.394(6) . ?
C1 C2 1.412(6) . ?
C2 C3 1.385(6) . ?
C2 H3 0.9500 . ?
C3 C4 1.411(7) . ?
C4 C5 1.371(6) . ?
C5 C6 1.417(6) . ?
C5 H4 0.9500 . ?
C7 C8 1.373(7) . ?
C9 C10 1.354(7) . ?
C11 C12 1.525(12) . ?
C11 H5 1.06(5) . ?
C11 H6 0.79(6) . ?
C12 H7 0.99(6) . ?
C12 H8 1.11(8) . ?
C13 C14 1.46(5) . ?
C13 H5 0.95(5) . ?
C13 H6 1.36(7) . ?
C14 H6 1.20(6) . ?
C14 H7 1.16(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
C7 S1 C1 95.4(2) . . ?
C7 S2 C6 95.2(2) . . ?
C8 S3 C9 94.8(2) . . ?
C8 S4 C10 95.2(2) . . ?
C9 S5 C13 103.9(9) . . ?
C9 S5 C11 102.3(3) . . ?
C10 S6 C12 99.8(3) . . ?
C10 S6 C14 101.3(12) . . ?
C3 O1 H1 111.7(11) . . ?
C4 O2 H2 118(5) . . ?
C6 C1 C2 121.0(4) . . ?
C6 C1 S1 116.1(4) . . ?
C2 C1 S1 122.9(4) . . ?
C3 C2 C1 118.6(4) . . ?
C3 C2 H3 120.7 . . ?
C1 C2 H3 120.7 . . ?
O1 C3 C2 121.6(4) . . ?
O1 C3 C4 117.7(4) . . ?
C2 C3 C4 120.7(4) . . ?
O2 C4 C5 117.6(4) . . ?
O2 C4 C3 121.9(4) . . ?
C5 C4 C3 120.4(4) . . ?
C4 C5 C6 119.9(4) . . ?
C4 C5 H4 120.0 . . ?
C6 C5 H4 120.0 . . ?
C1 C6 C5 119.3(4) . . ?
C1 C6 S2 117.0(4) . . ?
C5 C6 S2 123.7(4) . . ?
C8 C7 S2 121.4(4) . . ?
C8 C7 S1 122.4(4) . . ?
S2 C7 S1 116.2(3) . . ?
C7 C8 S3 122.2(4) . . ?
C7 C8 S4 122.1(4) . . ?
S3 C8 S4 115.7(3) . . ?
C10 C9 S3 117.8(4) . . ?
C10 C9 S5 128.6(4) . . ?
S3 C9 S5 113.5(3) . . ?
C9 C10 S6 128.2(4) . . ?
C9 C10 S4 116.3(4) . . ?
S6 C10 S4 115.5(3) . . ?
C12 C11 S5 114.2(6) . . ?
C12 C11 H5 109(3) . . ?
S5 C11 H5 102(2) . . ?
C12 C11 H6 105(5) . . ?
S5 C11 H6 107(5) . . ?
H5 C11 H6 120(5) . . ?
C11 C12 S6 113.8(6) . . ?
C11 C12 H7 106(3) . . ?
S6 C12 H7 100(3) . . ?
C11 C12 H8 109(4) . . ?
S6 C12 H8 114(4) . . ?
H7 C12 H8 113(5) . . ?
C14 C13 S5 114(3) . . ?
C14 C13 H5 114(4) . . ?
S5 C13 H5 107(4) . . ?
C14 C13 H6 50(3) . . ?
S5 C13 H6 85(3) . . ?
H5 C13 H6 86(5) . . ?
C13 C14 S6 121(3) . . ?
C13 C14 H6 61(3) . . ?
S6 C14 H6 130(4) . . ?
C13 C14 H7 99(4) . . ?
S6 C14 H7 91(4) . . ?
H6 C14 H7 138(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
C7 S1 C1 C6 1.6(4) . . . . ?
C7 S1 C1 C2 -178.0(4) . . . . ?
C6 C1 C2 C3 0.6(7) . . . . ?
S1 C1 C2 C3 -179.8(3) . . . . ?
C1 C2 C3 O1 -177.9(4) . . . . ?
C1 C2 C3 C4 1.4(7) . . . . ?
O1 C3 C4 O2 0.7(7) . . . . ?
C2 C3 C4 O2 -178.7(4) . . . . ?
O1 C3 C4 C5 176.6(4) . . . . ?
C2 C3 C4 C5 -2.8(7) . . . . ?
O2 C4 C5 C6 178.1(4) . . . . ?
C3 C4 C5 C6 2.0(7) . . . . ?
C2 C1 C6 C5 -1.3(6) . . . . ?
S1 C1 C6 C5 179.1(3) . . . . ?
C2 C1 C6 S2 177.6(3) . . . . ?
S1 C1 C6 S2 -2.0(5) . . . . ?
C4 C5 C6 C1 0.0(7) . . . . ?
C4 C5 C6 S2 -178.9(3) . . . . ?
C7 S2 C6 C1 1.3(4) . . . . ?
C7 S2 C6 C5 -179.8(4) . . . . ?
C6 S2 C7 C8 179.7(4) . . . . ?
C6 S2 C7 S1 -0.2(3) . . . . ?
C1 S1 C7 C8 179.5(4) . . . . ?
C1 S1 C7 S2 -0.7(3) . . . . ?
S2 C7 C8 S3 -178.2(3) . . . . ?
S1 C7 C8 S3 1.6(6) . . . . ?
S2 C7 C8 S4 1.2(6) . . . . ?
S1 C7 C8 S4 -178.9(3) . . . . ?
C9 S3 C8 C7 177.1(4) . . . . ?
C9 S3 C8 S4 -2.4(3) . . . . ?
C10 S4 C8 C7 -176.4(4) . . . . ?
C10 S4 C8 S3 3.2(3) . . . . ?
C8 S3 C9 C10 0.3(4) . . . . ?
C8 S3 C9 S5 -178.6(3) . . . . ?
C13 S5 C9 C10 -13.0(14) . . . . ?
C11 S5 C9 C10 5.6(7) . . . . ?
C13 S5 C9 S3 165.8(13) . . . . ?
C11 S5 C9 S3 -175.6(5) . . . . ?
S3 C9 C10 S6 -178.7(3) . . . . ?
S5 C9 C10 S6 0.0(7) . . . . ?
S3 C9 C10 S4 1.9(5) . . . . ?
S5 C9 C10 S4 -179.4(3) . . . . ?
C12 S6 C10 C9 20.8(6) . . . . ?
C14 S6 C10 C9 -9.0(16) . . . . ?
C12 S6 C10 S4 -159.7(4) . . . . ?
C14 S6 C10 S4 170.4(15) . . . . ?
C8 S4 C10 C9 -3.0(4) . . . . ?
C8 S4 C10 S6 177.5(3) . . . . ?
C9 S5 C11 C12 -39.5(9) . . . . ?
S5 C11 C12 S6 69.7(10) . . . . ?
C10 S6 C12 C11 -54.7(7) . . . . ?
C9 S5 C13 C14 41(3) . . . . ?
S5 C13 C14 S6 -61(5) . . . . ?
C10 S6 C14 C13 41(4) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O2 H2 O1 . . . 2.757(5) 0.86(8) 2.60(8) 91(6) no
O2 H2 O1 . . 5_656 2.616(5) 0.86(8) 1.78(8) 165(9) no

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.


####################################################################### 
# 
# 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_H-TTF_270K
_database_code_depnum_ccdc_archive 'CCDC 1896678'
loop_
_audit_author_name
_audit_author_address
'Akira Ueda'
;Kumamoto University
Japan
;
_audit_update_record             
;
2019-05-20 deposited with the CCDC.	2019-06-04 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C24 H15 O4 S12'
_chemical_formula_moiety         'C24 H15 O4 S12'
_chemical_formula_weight         752.10
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
_space_group_IT_number           15
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                   29.348(3)
_cell_length_b                   8.4654(3)
_cell_length_c                   11.2565(4)
_cell_angle_alpha                90.0000
_cell_angle_beta                 100.911(6)
_cell_angle_gamma                90.0000
_cell_volume                     2746.0(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5281
_cell_measurement_theta_min      1.99
_cell_measurement_theta_max      37.01
_cell_measurement_temperature    270
#------------------------------------------------------------------------------
_exptl_crystal_description       platelet
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.003
_exptl_crystal_density_diffrn    1.819
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1532.00
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_correction_type   none

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      270
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     1.00000
_diffrn_measurement_device_type  'Rigaku Imaging Plate'
_diffrn_reflns_number            4385
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_av_R_equivalents  0.0569
_diffrn_reflns_theta_max         37.025
_diffrn_reflns_theta_min         1.989
_diffrn_reflns_theta_full        36.870
_diffrn_measured_fraction_theta_max 0.891
_diffrn_measured_fraction_theta_full 0.893
_diffrn_reflns_Laue_measured_fraction_max 0.891
_diffrn_reflns_Laue_measured_fraction_full 0.893
_diffrn_reflns_point_group_measured_fraction_max 0.891
_diffrn_reflns_point_group_measured_fraction_full 0.893
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             2241
_reflns_number_gt                1856
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0546
_refine_ls_wR_factor_ref         0.1461
_refine_ls_wR_factor_gt          0.1419
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_reflns         2241
_refine_ls_number_parameters     202
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.1144P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.000
_refine_diff_density_max         0.45
_refine_diff_density_min         -0.50
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
O O 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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
S1 S 0.31844(3) -0.02016(10) 0.10349(8) 0.0357(3) Uani 1 1 d . . . . .
S2 S 0.29265(3) 0.21086(10) 0.27636(8) 0.0368(3) Uani 1 1 d . . . . .
S3 S 0.21291(3) -0.01688(11) -0.04480(9) 0.0374(3) Uani 1 1 d . . . . .
S4 S 0.18849(3) 0.21929(10) 0.12501(8) 0.0370(3) Uani 1 1 d . . . . .
S5 S 0.11943(3) -0.04954(11) -0.18934(9) 0.0400(3) Uani 1 1 d . . . . .
S6 S 0.08857(3) 0.22687(12) 0.01643(9) 0.0468(3) Uani 1 1 d . . . . .
O1 O 0.48614(8) -0.0051(3) 0.3478(2) 0.0428(6) Uani 1 1 d . . . . .
O2 O 0.45958(9) 0.2022(3) 0.5119(2) 0.0413(6) Uani 1 1 d . . . . .
C1 C 0.36278(11) 0.0393(4) 0.2219(3) 0.0310(7) Uani 1 1 d . . . . .
C2 C 0.40838(11) -0.0139(4) 0.2355(3) 0.0325(8) Uani 1 1 d . . . . .
H3 H 0.416626 -0.084899 0.180219 0.039 Uiso 1 1 calc R U . . .
C3 C 0.44150(11) 0.0395(4) 0.3319(3) 0.0325(8) Uani 1 1 d . . . . .
C4 C 0.42791(10) 0.1446(4) 0.4166(3) 0.0315(7) Uani 1 1 d . . . . .
C5 C 0.38307(11) 0.1991(4) 0.4022(3) 0.0326(8) Uani 1 1 d . . . . .
H4 H 0.374726 0.270136 0.457406 0.039 Uiso 1 1 calc R U . . .
C6 C 0.35023(10) 0.1467(4) 0.3040(3) 0.0302(7) Uani 1 1 d . . . . .
C7 C 0.27563(11) 0.0967(4) 0.1476(3) 0.0332(7) Uani 1 1 d . . . . .
C8 C 0.23117(11) 0.1003(4) 0.0828(3) 0.0331(7) Uani 1 1 d . . . . .
C9 C 0.15490(11) 0.0424(4) -0.0665(3) 0.0332(8) Uani 1 1 d . . . . .
C10 C 0.14342(10) 0.1482(4) 0.0126(3) 0.0342(8) Uani 1 1 d . . . . .
C11 C 0.0648(2) 0.0545(10) -0.1953(7) 0.0429(18) Uiso 0.676(15) 1 d . . P A 1
C12 C 0.05294(19) 0.0841(7) -0.0680(5) 0.040(2) Uiso 0.676(15) 1 d . . P A 1
C13 C 0.0612(4) -0.0029(18) -0.1652(13) 0.036(3) Uiso 0.324(15) 1 d . . P A 2
C14 C 0.0562(5) 0.1588(18) -0.1303(14) 0.058(5) Uiso 0.324(15) 1 d . . P A 2
H1 H 0.500000 -0.019(8) 0.250000 0.09(2) Uiso 1 2 d S . P . .
H2 H 0.4782(15) 0.134(5) 0.533(4) 0.058(14) Uiso 1 1 d . . . . .
H5 H 0.0459(16) -0.043(6) -0.230(5) 0.072(15) Uiso 1 1 d . . . . .
H6 H 0.0640(19) 0.159(7) -0.228(5) 0.105(18) Uiso 1 1 d . . . . .
H7 H 0.0195(17) 0.125(6) -0.092(4) 0.085(15) Uiso 1 1 d . . . . .
H8 H 0.0519(15) -0.018(5) -0.039(4) 0.061(12) Uiso 1 1 d . . . . .


#==============================================================================
_computing_data_collection       PROCESS-AUTO
_computing_cell_refinement       PROCESS-AUTO
_computing_data_reduction        PROCESS-AUTO
_computing_structure_solution    'SIR2014 (Burla, et al., 2014)'
_computing_structure_refinement  'SHELXL Version 2018/3 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2019)'
_computing_molecular_graphics    'CrystalStructure 4.3'

#==============================================================================
# MOLECULAR GEOMETRY

_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
S1 C7 1.744(3) . ?
S1 C1 1.751(3) . ?
S2 C7 1.735(3) . ?
S2 C6 1.746(3) . ?
S3 C8 1.744(3) . ?
S3 C9 1.747(3) . ?
S4 C8 1.742(3) . ?
S4 C10 1.755(3) . ?
S5 C9 1.748(4) . ?
S5 C11 1.820(6) . ?
S5 C13 1.823(12) . ?
S6 C10 1.750(3) . ?
S6 C12 1.755(6) . ?
S6 C14 1.835(15) . ?
O1 C3 1.342(4) . ?
O1 H1 1.250(7) . ?
O2 C4 1.369(4) . ?
O2 H2 0.80(4) . ?
C1 C2 1.393(4) . ?
C1 C6 1.395(4) . ?
C2 C3 1.387(5) . ?
C2 H3 0.9300 . ?
C3 C4 1.417(5) . ?
C4 C5 1.375(4) . ?
C5 C6 1.395(5) . ?
C5 H4 0.9300 . ?
C7 C8 1.369(5) . ?
C9 C10 1.350(5) . ?
C11 C12 1.557(9) . ?
C11 H5 1.03(5) . ?
C11 H6 0.96(6) . ?
C12 H7 1.03(5) . ?
C12 H8 0.93(4) . ?
C13 C14 1.44(2) . ?
C13 H5 0.85(5) . ?
C13 H6 1.55(6) . ?
C13 H8 1.51(5) . ?
C14 H6 1.17(6) . ?
C14 H7 1.27(5) . ?

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
C7 S1 C1 95.28(15) . . ?
C7 S2 C6 95.24(15) . . ?
C8 S3 C9 95.24(15) . . ?
C8 S4 C10 95.04(15) . . ?
C9 S5 C11 101.7(2) . . ?
C9 S5 C13 102.7(4) . . ?
C10 S6 C12 100.4(2) . . ?
C10 S6 C14 100.4(4) . . ?
C3 O1 H1 112.4(9) . . ?
C4 O2 H2 107(3) . . ?
C2 C1 C6 120.4(3) . . ?
C2 C1 S1 123.5(3) . . ?
C6 C1 S1 116.1(2) . . ?
C3 C2 C1 119.9(3) . . ?
C3 C2 H3 120.1 . . ?
C1 C2 H3 120.1 . . ?
O1 C3 C2 122.3(3) . . ?
O1 C3 C4 118.6(3) . . ?
C2 C3 C4 119.1(3) . . ?
O2 C4 C5 117.8(3) . . ?
O2 C4 C3 121.0(3) . . ?
C5 C4 C3 121.1(3) . . ?
C4 C5 C6 119.3(3) . . ?
C4 C5 H4 120.4 . . ?
C6 C5 H4 120.4 . . ?
C1 C6 C5 120.2(3) . . ?
C1 C6 S2 116.9(2) . . ?
C5 C6 S2 122.9(2) . . ?
C8 C7 S2 121.8(3) . . ?
C8 C7 S1 121.7(3) . . ?
S2 C7 S1 116.41(18) . . ?
C7 C8 S4 122.0(3) . . ?
C7 C8 S3 122.6(3) . . ?
S4 C8 S3 115.38(18) . . ?
C10 C9 S5 129.2(3) . . ?
C10 C9 S3 117.1(3) . . ?
S5 C9 S3 113.66(19) . . ?
C9 C10 S6 127.9(3) . . ?
C9 C10 S4 117.1(2) . . ?
S6 C10 S4 115.04(19) . . ?
C12 C11 S5 113.1(5) . . ?
C12 C11 H5 106(3) . . ?
S5 C11 H5 92(2) . . ?
C12 C11 H6 102(4) . . ?
S5 C11 H6 115(4) . . ?
H5 C11 H6 128(4) . . ?
C11 C12 S6 113.3(4) . . ?
C11 C12 H7 101(3) . . ?
S6 C12 H7 111(3) . . ?
C11 C12 H8 102(3) . . ?
S6 C12 H8 120(3) . . ?
H7 C12 H8 108(4) . . ?
C14 C13 S5 113.2(10) . . ?
C14 C13 H5 123(4) . . ?
S5 C13 H5 98(3) . . ?
C14 C13 H6 46(2) . . ?
S5 C13 H6 90(2) . . ?
H5 C13 H6 91(4) . . ?
C14 C13 H8 77.0(19) . . ?
S5 C13 H8 117.8(19) . . ?
H5 C13 H8 128(4) . . ?
H6 C13 H8 123(3) . . ?
C13 C14 S6 118.8(12) . . ?
C13 C14 H6 72(3) . . ?
S6 C14 H6 134(3) . . ?
C13 C14 H7 91(2) . . ?
S6 C14 H7 95(2) . . ?
H6 C14 H7 131(4) . . ?

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
C7 S1 C1 C2 -178.5(3) . . . . ?
C7 S1 C1 C6 0.8(3) . . . . ?
C6 C1 C2 C3 0.5(5) . . . . ?
S1 C1 C2 C3 179.8(2) . . . . ?
C1 C2 C3 O1 -178.5(3) . . . . ?
C1 C2 C3 C4 1.5(5) . . . . ?
O1 C3 C4 O2 1.1(5) . . . . ?
C2 C3 C4 O2 -178.9(3) . . . . ?
O1 C3 C4 C5 177.4(3) . . . . ?
C2 C3 C4 C5 -2.6(5) . . . . ?
O2 C4 C5 C6 178.0(3) . . . . ?
C3 C4 C5 C6 1.6(5) . . . . ?
C2 C1 C6 C5 -1.5(5) . . . . ?
S1 C1 C6 C5 179.1(2) . . . . ?
C2 C1 C6 S2 178.0(2) . . . . ?
S1 C1 C6 S2 -1.3(3) . . . . ?
C4 C5 C6 C1 0.5(5) . . . . ?
C4 C5 C6 S2 -179.1(2) . . . . ?
C7 S2 C6 C1 1.1(3) . . . . ?
C7 S2 C6 C5 -179.4(3) . . . . ?
C6 S2 C7 C8 -179.4(3) . . . . ?
C6 S2 C7 S1 -0.5(2) . . . . ?
C1 S1 C7 C8 178.8(3) . . . . ?
C1 S1 C7 S2 -0.1(2) . . . . ?
S2 C7 C8 S4 -0.1(4) . . . . ?
S1 C7 C8 S4 -178.92(18) . . . . ?
S2 C7 C8 S3 -178.42(18) . . . . ?
S1 C7 C8 S3 2.8(4) . . . . ?
C10 S4 C8 C7 -175.2(3) . . . . ?
C10 S4 C8 S3 3.2(2) . . . . ?
C9 S3 C8 C7 176.1(3) . . . . ?
C9 S3 C8 S4 -2.3(2) . . . . ?
C11 S5 C9 C10 7.4(5) . . . . ?
C13 S5 C9 C10 -12.3(7) . . . . ?
C11 S5 C9 S3 -173.7(3) . . . . ?
C13 S5 C9 S3 166.5(6) . . . . ?
C8 S3 C9 C10 0.1(3) . . . . ?
C8 S3 C9 S5 -178.90(19) . . . . ?
S5 C9 C10 S6 0.0(5) . . . . ?
S3 C9 C10 S6 -178.8(2) . . . . ?
S5 C9 C10 S4 -179.0(2) . . . . ?
S3 C9 C10 S4 2.2(4) . . . . ?
C12 S6 C10 C9 20.3(4) . . . . ?
C14 S6 C10 C9 -11.2(6) . . . . ?
C12 S6 C10 S4 -160.6(3) . . . . ?
C14 S6 C10 S4 167.9(5) . . . . ?
C8 S4 C10 C9 -3.2(3) . . . . ?
C8 S4 C10 S6 177.6(2) . . . . ?
C9 S5 C11 C12 -41.4(6) . . . . ?
S5 C11 C12 S6 71.2(6) . . . . ?
C10 S6 C12 C11 -54.8(5) . . . . ?
C9 S5 C13 C14 43.6(13) . . . . ?
S5 C13 C14 S6 -66.0(15) . . . . ?
C10 S6 C14 C13 46.1(12) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O2 H2 O1 . . . 2.765(4) 0.80(4) 2.44(5) 106(3) no
O2 H2 O1 . . 5_656 2.620(3) 0.80(4) 1.89(4) 152(5) no

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.


####################################################################### 
# 
# 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_H-TTF_235K
_database_code_depnum_ccdc_archive 'CCDC 1896675'
loop_
_audit_author_name
_audit_author_address
'Akira Ueda'
;Kumamoto University
Japan
;
_audit_update_record             
;
2019-05-20 deposited with the CCDC.	2019-06-04 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C24 H15 O4 S12'
_chemical_formula_moiety         'C24 H15 O4 S12'
_chemical_formula_weight         752.10
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
_space_group_IT_number           15
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                   29.35(2)
_cell_length_b                   8.450(6)
_cell_length_c                   11.225(9)
_cell_angle_alpha                90.0000
_cell_angle_beta                 101.005(11)
_cell_angle_gamma                90.0000
_cell_volume                     2733(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2838
_cell_measurement_theta_min      3.04
_cell_measurement_theta_max      27.49
_cell_measurement_temperature    235
#------------------------------------------------------------------------------
_exptl_crystal_description       platelet
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.003
_exptl_crystal_density_diffrn    1.828
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1532.00
_exptl_absorpt_coefficient_mu    0.995
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_absorpt_correction_T_min  0.791
_exptl_absorpt_correction_T_max  1.000

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      235
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 7.314
_diffrn_reflns_number            10339
_diffrn_reflns_av_unetI/netI     0.0731
_diffrn_reflns_av_R_equivalents  0.0686
_diffrn_reflns_theta_max         27.460
_diffrn_reflns_theta_min         3.038
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             3079
_reflns_number_gt                1895
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.1204
_refine_ls_R_factor_gt           0.0705
_refine_ls_wR_factor_ref         0.1880
_refine_ls_wR_factor_gt          0.1567
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_reflns         3079
_refine_ls_number_parameters     202
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0883P)²+3.5191P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.000
_refine_diff_density_max         0.46
_refine_diff_density_min         -0.42
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.1246 0.1234
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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
S1 S 0.18146(5) -0.01993(16) 0.39648(12) 0.0369(4) Uani 1 1 d . . . . .
S2 S 0.20743(5) 0.21136(17) 0.22327(12) 0.0364(4) Uani 1 1 d . . . . .
S3 S 0.28693(5) -0.01672(17) 0.54496(13) 0.0384(4) Uani 1 1 d . . . . .
S4 S 0.31150(5) 0.21987(17) 0.37464(12) 0.0371(4) Uani 1 1 d . . . . .
S5 S 0.38045(5) -0.04921(17) 0.68949(13) 0.0408(4) Uani 1 1 d . . . . .
S6 S 0.41124(5) 0.22757(19) 0.48386(14) 0.0474(4) Uani 1 1 d . . . . .
O1 O 0.01387(12) -0.0032(5) 0.1520(3) 0.0422(9) Uani 1 1 d . . . . .
O2 O 0.04013(13) 0.2023(5) -0.0130(3) 0.0409(10) Uani 1 1 d . . . . .
C1 C 0.13764(17) 0.0399(5) 0.2793(4) 0.0296(11) Uani 1 1 d . . . . .
C2 C 0.09131(17) -0.0134(6) 0.2643(4) 0.0301(11) Uani 1 1 d . . . . .
H3 H 0.082683 -0.085094 0.320048 0.036 Uiso 1 1 calc R U . . .
C3 C 0.05872(17) 0.0402(6) 0.1674(5) 0.0338(12) Uani 1 1 d . . . . .
C4 C 0.07174(18) 0.1452(6) 0.0827(5) 0.0333(12) Uani 1 1 d . . . . .
C5 C 0.11657(17) 0.1999(6) 0.0965(5) 0.0325(12) Uani 1 1 d . . . . .
H4 H 0.124840 0.271863 0.040424 0.039 Uiso 1 1 calc R U . . .
C6 C 0.14993(17) 0.1471(6) 0.1957(4) 0.0309(11) Uani 1 1 d . . . . .
C7 C 0.22436(17) 0.0972(6) 0.3532(5) 0.0338(12) Uani 1 1 d . . . . .
C8 C 0.26879(18) 0.1005(6) 0.4168(5) 0.0370(13) Uani 1 1 d . . . . .
C9 C 0.34501(18) 0.0426(6) 0.5669(5) 0.0330(12) Uani 1 1 d . . . . .
C10 C 0.35653(18) 0.1475(6) 0.4871(5) 0.0358(12) Uani 1 1 d . . . . .
C11 C 0.4347(3) 0.0486(16) 0.6943(10) 0.039(3) Uiso 0.69(3) 1 d . . P A 1
C12 C 0.4468(3) 0.0819(12) 0.5685(9) 0.039(3) Uiso 0.69(3) 1 d . . P A 1
C13 C 0.4396(9) -0.006(4) 0.669(3) 0.054(8) Uiso 0.31(3) 1 d . . P A 2
C14 C 0.4448(9) 0.154(3) 0.627(3) 0.066(10) Uiso 0.31(3) 1 d . . P A 2
H1 H 0.000000 0.002(14) 0.250000 0.12(4) Uiso 1 2 d S . P . .
H2 H 0.020(3) 0.121(8) -0.049(7) 0.09(3) Uiso 1 1 d . . . . .
H5 H 0.4600(18) -0.027(6) 0.753(5) 0.040(15) Uiso 1 1 d . . . . .
H6 H 0.433(2) 0.142(8) 0.724(6) 0.06(2) Uiso 1 1 d . . . . .
H7 H 0.445(2) -0.022(8) 0.538(6) 0.07(2) Uiso 1 1 d . . . . .
H8 H 0.476(2) 0.134(8) 0.582(6) 0.07(2) Uiso 1 1 d . . . . .


#==============================================================================
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       CrystalClear
_computing_data_reduction        CrystalClear
_computing_structure_solution    'SIR2014 (Burla, et al., 2014)'
_computing_structure_refinement  'SHELXL Version 2018/3 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2019)'
_computing_molecular_graphics    'CrystalStructure 4.3'

#==============================================================================
# MOLECULAR GEOMETRY

_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
S1 C1 1.731(5) . ?
S1 C7 1.742(5) . ?
S2 C7 1.740(5) . ?
S2 C6 1.743(5) . ?
S3 C8 1.744(6) . ?
S3 C9 1.749(5) . ?
S4 C8 1.743(5) . ?
S4 C10 1.754(5) . ?
S5 C9 1.741(5) . ?
S5 C11 1.786(10) . ?
S5 C13 1.83(2) . ?
S6 C10 1.749(5) . ?
S6 C12 1.769(9) . ?
S6 C14 1.83(3) . ?
O1 C3 1.346(6) . ?
O1 H1 1.244(5) . ?
O2 C4 1.366(6) . ?
O2 H2 0.94(7) . ?
C1 C6 1.399(7) . ?
C1 C2 1.412(7) . ?
C2 C3 1.380(7) . ?
C2 H3 0.9400 . ?
C3 C4 1.406(7) . ?
C4 C5 1.375(7) . ?
C5 C6 1.408(7) . ?
C5 H4 0.9400 . ?
C7 C8 1.362(7) . ?
C9 C10 1.348(7) . ?
C11 C12 1.547(15) . ?
C11 H5 1.10(5) . ?
C11 H6 0.86(6) . ?
C12 H7 0.94(7) . ?
C12 H8 0.94(7) . ?
C13 C14 1.45(4) . ?
C13 H5 1.03(6) . ?
C13 H6 1.42(7) . ?
C14 H6 1.21(6) . ?
C14 H8 1.13(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
C1 S1 C7 95.4(2) . . ?
C7 S2 C6 95.0(2) . . ?
C8 S3 C9 95.1(2) . . ?
C8 S4 C10 94.9(3) . . ?
C9 S5 C11 102.3(4) . . ?
C9 S5 C13 104.6(8) . . ?
C10 S6 C12 99.8(4) . . ?
C10 S6 C14 101.1(8) . . ?
C3 O1 H1 110.8(17) . . ?
C4 O2 H2 111(4) . . ?
C6 C1 C2 119.5(4) . . ?
C6 C1 S1 116.7(4) . . ?
C2 C1 S1 123.8(4) . . ?
C3 C2 C1 119.7(5) . . ?
C3 C2 H3 120.1 . . ?
C1 C2 H3 120.1 . . ?
O1 C3 C2 121.7(5) . . ?
O1 C3 C4 118.1(5) . . ?
C2 C3 C4 120.2(5) . . ?
O2 C4 C5 117.5(5) . . ?
O2 C4 C3 121.6(5) . . ?
C5 C4 C3 120.9(5) . . ?
C4 C5 C6 119.3(5) . . ?
C4 C5 H4 120.4 . . ?
C6 C5 H4 120.4 . . ?
C1 C6 C5 120.4(5) . . ?
C1 C6 S2 116.6(4) . . ?
C5 C6 S2 123.0(4) . . ?
C8 C7 S1 122.4(4) . . ?
C8 C7 S2 121.3(4) . . ?
S1 C7 S2 116.3(3) . . ?
C7 C8 S3 122.1(4) . . ?
C7 C8 S4 122.4(4) . . ?
S3 C8 S4 115.5(3) . . ?
C10 C9 S5 129.1(4) . . ?
C10 C9 S3 117.2(4) . . ?
S5 C9 S3 113.7(3) . . ?
C9 C10 S6 128.0(4) . . ?
C9 C10 S4 117.2(4) . . ?
S6 C10 S4 114.8(3) . . ?
C12 C11 S5 114.6(8) . . ?
C12 C11 H5 114(3) . . ?
S5 C11 H5 104(3) . . ?
C12 C11 H6 103(4) . . ?
S5 C11 H6 108(4) . . ?
H5 C11 H6 113(5) . . ?
C11 C12 S6 113.7(8) . . ?
C11 C12 H7 99(4) . . ?
S6 C12 H7 118(4) . . ?
C11 C12 H8 107(4) . . ?
S6 C12 H8 101(4) . . ?
H7 C12 H8 119(6) . . ?
C14 C13 S5 113(2) . . ?
C14 C13 H5 112(4) . . ?
S5 C13 H5 105(4) . . ?
C14 C13 H6 50(3) . . ?
S5 C13 H6 84(3) . . ?
H5 C13 H6 82(4) . . ?
C13 C14 S6 122(2) . . ?
C13 C14 H6 64(4) . . ?
S6 C14 H6 128(4) . . ?
C13 C14 H8 98(4) . . ?
S6 C14 H8 90(4) . . ?
H6 C14 H8 142(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
C7 S1 C1 C6 1.6(4) . . . . ?
C7 S1 C1 C2 -178.6(4) . . . . ?
C6 C1 C2 C3 0.2(7) . . . . ?
S1 C1 C2 C3 -179.6(4) . . . . ?
C1 C2 C3 O1 -177.6(4) . . . . ?
C1 C2 C3 C4 1.2(7) . . . . ?
O1 C3 C4 O2 -0.1(7) . . . . ?
C2 C3 C4 O2 -178.9(5) . . . . ?
O1 C3 C4 C5 176.9(5) . . . . ?
C2 C3 C4 C5 -2.0(8) . . . . ?
O2 C4 C5 C6 178.4(4) . . . . ?
C3 C4 C5 C6 1.4(8) . . . . ?
C2 C1 C6 C5 -0.8(7) . . . . ?
S1 C1 C6 C5 179.0(4) . . . . ?
C2 C1 C6 S2 178.2(4) . . . . ?
S1 C1 C6 S2 -2.0(5) . . . . ?
C4 C5 C6 C1 0.0(7) . . . . ?
C4 C5 C6 S2 -178.9(4) . . . . ?
C7 S2 C6 C1 1.3(4) . . . . ?
C7 S2 C6 C5 -179.8(4) . . . . ?
C1 S1 C7 C8 179.2(5) . . . . ?
C1 S1 C7 S2 -0.7(3) . . . . ?
C6 S2 C7 C8 180.0(5) . . . . ?
C6 S2 C7 S1 -0.2(3) . . . . ?
S1 C7 C8 S3 1.8(7) . . . . ?
S2 C7 C8 S3 -178.3(3) . . . . ?
S1 C7 C8 S4 -179.0(3) . . . . ?
S2 C7 C8 S4 0.8(7) . . . . ?
C9 S3 C8 C7 176.7(5) . . . . ?
C9 S3 C8 S4 -2.4(3) . . . . ?
C10 S4 C8 C7 -175.5(5) . . . . ?
C10 S4 C8 S3 3.6(4) . . . . ?
C11 S5 C9 C10 6.8(7) . . . . ?
C13 S5 C9 C10 -11.9(12) . . . . ?
C11 S5 C9 S3 -175.1(5) . . . . ?
C13 S5 C9 S3 166.3(11) . . . . ?
C8 S3 C9 C10 -0.3(5) . . . . ?
C8 S3 C9 S5 -178.7(3) . . . . ?
S5 C9 C10 S6 -1.3(8) . . . . ?
S3 C9 C10 S6 -179.4(3) . . . . ?
S5 C9 C10 S4 -179.0(3) . . . . ?
S3 C9 C10 S4 3.0(6) . . . . ?
C12 S6 C10 C9 21.7(6) . . . . ?
C14 S6 C10 C9 -8.0(12) . . . . ?
C12 S6 C10 S4 -160.6(4) . . . . ?
C14 S6 C10 S4 169.7(11) . . . . ?
C8 S4 C10 C9 -3.9(5) . . . . ?
C8 S4 C10 S6 178.1(3) . . . . ?
C9 S5 C11 C12 -39.6(10) . . . . ?
S5 C11 C12 S6 69.4(11) . . . . ?
C10 S6 C12 C11 -54.0(8) . . . . ?
C9 S5 C13 C14 40(3) . . . . ?
S5 C13 C14 S6 -60(3) . . . . ?
C10 S6 C14 C13 41(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O2 H2 O1 . . . 2.755(6) 0.94(7) 2.53(8) 94(5) no
O2 H2 O1 . . 5_555 2.614(5) 0.94(7) 1.70(7) 163(7) no

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.


