# Electronic Supplementary Material (ESI) for Materials Advances.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_exp_1964_auto
_database_code_depnum_ccdc_archive 'CCDC 2296888'
loop_
_audit_author_name
_audit_author_address
'Narcis Avarvari'
;CNRS University of Angers
France
;
_audit_update_record             
;
2023-09-22 deposited with the CCDC.	2024-01-30 downloaded from the CCDC.
;
_audit_creation_date             2023-07-06
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
nicolas.zigon@univ-angers.fr
_chemical_name_common            ?
_chemical_name_systematic        BVDTTTF(PF6)
_chemical_formula_moiety         'F6 Ta, C10 H4 S8'
_chemical_formula_sum            'C10 H4 F6 S8 Ta'
_chemical_formula_weight         675.56
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C10 H4 S8 Ta2 F10 O1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ta Ta -5.7959 5.2718 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           58
_space_group_name_H-M_alt        'P n n m'
_space_group_name_Hall           '-P 2 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'x-1/2, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   4.8259(3)
_cell_length_b                   17.8935(9)
_cell_length_c                   10.1805(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     879.11(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1320
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      71.6790
_cell_measurement_theta_min      4.9320
_shelx_estimated_absorpt_T_max   0.420
_shelx_estimated_absorpt_T_min   0.057
_exptl_absorpt_coefficient_mu    20.964
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.11148
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.118a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.552
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             638
_exptl_crystal_preparation       electrocrystallization
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max          0.319
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            1810
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.803
_diffrn_reflns_theta_min         4.943
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1990
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      1.00  28.00   1.00   45.00    --  -42.94  19.00  30.00   27
  2  ω      1.00  31.00   1.00   45.00    --  -42.94  19.00-180.00   30
  3  ω     -9.00  24.00   1.00   45.00    --   42.94 -19.00 -60.00   33
  4  ω     -7.00  24.00   1.00   45.00    --   42.94 -19.00-150.00   31
  5  ω     97.00 140.00   1.00  180.00    --  103.00  77.00 -90.00   43
  6  ω    111.00 158.00   1.00  180.00    --  103.00  30.00  60.00   47
  7  ω     78.00 149.00   1.00  180.00    --  103.00 125.00 150.00   71
  8  ω     35.00  66.00   1.00  180.00    --  103.00 -58.00 -67.00   31
  9  ω     30.00  82.00   1.00  180.00    --  103.00 -77.00 120.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'SuperNova, Single source at offset/far, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.2210993000
_diffrn_orient_matrix_UB_12      0.0175417000
_diffrn_orient_matrix_UB_13      -0.1047484000
_diffrn_orient_matrix_UB_21      0.0117560000
_diffrn_orient_matrix_UB_22      -0.0834083000
_diffrn_orient_matrix_UB_23      -0.0373094000
_diffrn_orient_matrix_UB_31      -0.2299062000
_diffrn_orient_matrix_UB_32      0.0125371000
_diffrn_orient_matrix_UB_33      -0.1025301000
_diffrn_oxdiff_digest_frames     
;
0197f084ceb09bd140fd0b14612580bd1d00027599c
;
_diffrn_oxdiff_digest_hkl        
;
0161ca7a0e7d6a4900d706b08206bf502d82e9
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                826
_reflns_number_total             883
_reflns_odcompleteness_completeness 98.05
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         2.169
_refine_diff_density_min         -1.305
_refine_diff_density_rms         0.210
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     62
_refine_ls_number_reflns         883
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0393
_refine_ls_restrained_S_all      1.099
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0851P)²+0.8058P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1129
_refine_ls_wR_factor_ref         0.1141
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C008(H008)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ta01 Ta 0.500000 0.000000 0.000000 0.0275(3) Uani 1 4 d S T P . .
S002 S 0.2140(3) 0.06886(6) 0.35662(11) 0.0307(3) Uani 1 1 d . . . . .
S003 S 0.6166(3) 0.19600(6) 0.33707(13) 0.0341(4) Uani 1 1 d . . . . .
F004 F 0.6567(10) 0.0618(2) 0.1325(4) 0.0621(12) Uani 1 1 d . . . . .
F005 F 0.1898(13) 0.0605(3) 0.000000 0.096(3) Uani 1 2 d S T P . .
C006 C 0.0932(16) 0.0299(4) 0.500000 0.0290(14) Uani 1 2 d S T P . .
C007 C 0.4301(11) 0.1329(3) 0.4339(6) 0.0270(10) Uani 1 1 d . . . . .
C008 C 0.5754(13) 0.2769(3) 0.4349(6) 0.0376(12) Uani 1 1 d . . . . .
H008 H 0.551790 0.323441 0.391290 0.045 Uiso 1 1 calc R . . . .


_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
Ta01 F004 1.902(4) 6 ?
Ta01 F004 1.902(4) 2_655 ?
Ta01 F004 1.902(4) 5_655 ?
Ta01 F004 1.902(4) . ?
Ta01 F005 1.848(6) 5_655 ?
Ta01 F005 1.848(6) . ?
S002 C006 1.719(4) . ?
S002 C007 1.737(5) . ?
S003 C007 1.748(5) . ?
S003 C008 1.769(6) . ?
C006 C006 1.399(14) 5_556 ?
C007 C007 1.346(11) 6_556 ?
C008 C008 1.325(13) 6_556 ?

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
F004 Ta01 F004 180.0 . 5_655 ?
F004 Ta01 F004 90.4(2) 5_655 2_655 ?
F004 Ta01 F004 89.6(2) . 2_655 ?
F004 Ta01 F004 90.4(2) . 6 ?
F004 Ta01 F004 180.0(2) 2_655 6 ?
F004 Ta01 F004 89.6(2) 5_655 6 ?
F005 Ta01 F004 88.9(2) 5_655 5_655 ?
F005 Ta01 F004 88.9(2) . . ?
F005 Ta01 F004 91.1(2) 5_655 6 ?
F005 Ta01 F004 91.1(2) . 5_655 ?
F005 Ta01 F004 91.1(2) 5_655 . ?
F005 Ta01 F004 88.9(2) 5_655 2_655 ?
F005 Ta01 F004 91.1(2) . 2_655 ?
F005 Ta01 F004 88.9(2) . 6 ?
F005 Ta01 F005 180.0 5_655 . ?
C006 S002 C007 94.9(3) . . ?
C007 S003 C008 98.8(3) . . ?
S002 C006 S002 116.2(4) . 6_556 ?
C006 C006 S002 121.9(2) 5_556 . ?
C006 C006 S002 121.9(2) 5_556 6_556 ?
S002 C007 S003 118.7(3) . . ?
C007 C007 S002 116.92(19) 6_556 . ?
C007 C007 S003 124.31(19) 6_556 . ?
C008 C008 S003 124.3(2) 6_556 . ?

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
C006 S002 C007 S003 -177.7(4) . . . . ?
C006 S002 C007 C007 -1.3(3) . . . 6_556 ?
C007 S002 C006 S002 2.1(5) . . . 6_556 ?
C007 S002 C006 C006 -178.0(9) . . . 5_556 ?
C007 S003 C008 C008 37.2(3) . . . 6_556 ?
C008 S003 C007 S002 138.9(3) . . . . ?
C008 S003 C007 C007 -37.2(3) . . . 6_556 ?


_olex2_exptl_crystal_mounting_method 'paraffin oil'
_olex2_submission_original_sample_id exp_1964
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.534
_oxdiff_exptl_absorpt_empirical_full_min 0.500
####################################################################### 
# 
# 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_exp_1983
_database_code_depnum_ccdc_archive 'CCDC 2296890'
loop_
_audit_author_name
_audit_author_address
'Narcis Avarvari'
;CNRS University of Angers
France
;
_audit_update_record             
;
2023-09-22 deposited with the CCDC.	2024-01-30 downloaded from the CCDC.
;
_audit_creation_date             2023-09-11
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
nicolas.zigon@univ-angers.fr
_chemical_name_common            ?
_chemical_name_systematic        (BVDT-TTF)2ReO4
_chemical_formula_moiety         '0.5(O4 Re), C10 H4 S8'
_chemical_formula_sum            'C10 H4 O2 Re0.50 S8'
_chemical_formula_weight         505.71
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C9 H4 S8 Re1 O4'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 1 2/m 1'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   33.133(3)
_cell_length_b                   12.1739(14)
_cell_length_c                   3.8263(6)
_cell_angle_alpha                90
_cell_angle_beta                 93.360(11)
_cell_angle_gamma                90
_cell_volume                     1540.7(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    892
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      70.9400
_cell_measurement_theta_min      2.6100
_shelx_estimated_absorpt_T_max   0.578
_shelx_estimated_absorpt_T_min   0.111
_exptl_absorpt_coefficient_mu    18.139
_exptl_absorpt_correction_T_max  0.660
_exptl_absorpt_correction_T_min  0.190
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.94a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    2.180
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             982
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 5 0 0.0517
1 -5 0 0.0475
1 -1 2 0.0887
-1 0 -2 0.1125
-1 0 0 0.0172
1 0 0 0.0172

_exptl_crystal_preparation       electrocrystallization
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max          0.216
_exptl_crystal_size_mid          0.099
_exptl_crystal_size_min          0.034
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-1.0035 4.9751 -0.0050 0.4245 0.2647 -0.3846
1.0035 -4.9751 0.0050 -0.4245 -0.2647 0.3846
0.9628 -0.9751 1.9946 -0.5045 -0.3199 -0.5580
-0.9620 -0.0203 -1.9937 0.4254 0.2597 0.6353
-0.9993 -0.0020 -0.0003 0.0292 -0.0362 0.0021
0.9993 0.0020 0.0003 -0.0292 0.0362 -0.0021

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_Laue_measured_fraction_full 0.810
_diffrn_reflns_Laue_measured_fraction_max 0.810
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            1714
_diffrn_reflns_point_group_measured_fraction_full 0.810
_diffrn_reflns_point_group_measured_fraction_max 0.810
_diffrn_reflns_theta_full        66.589
_diffrn_reflns_theta_max         66.589
_diffrn_reflns_theta_min         2.672
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1990
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.810
_diffrn_measured_fraction_theta_max 0.810
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -12.00  31.00   1.00   40.00    --  -42.94  19.00  90.00   43
  2  ω     -9.00  23.00   1.00   40.00    --   42.94 -19.00  60.00   32
  3  ω    -31.00  24.00   1.00   40.00    --   42.94 -19.00-150.00   55
  4  ω    130.00 156.00   1.00  160.00    --  103.00 125.00 150.00   26
  5  ω     33.00  64.00   1.00  160.00    --  103.00 -61.00 -30.00   31
  6  ω     34.00  60.00   1.00  160.00    --  103.00 -61.00 150.00   26
  7  ω     37.00  63.00   1.00  160.00    --  103.00 -61.00-180.00   26
  8  ω     73.00 158.00   1.00  160.00    --  103.00  15.00-150.00   85
  9  ω     80.00 158.00   1.00  160.00    --  103.00  15.00 120.00   78
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'SuperNova, Single source at offset/far, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0293403000
_diffrn_orient_matrix_UB_12      0.0791994000
_diffrn_orient_matrix_UB_13      -0.2000451000
_diffrn_orient_matrix_UB_21      0.0361890000
_diffrn_orient_matrix_UB_22      0.0603614000
_diffrn_orient_matrix_UB_23      -0.1483287000
_diffrn_orient_matrix_UB_31      -0.0018634000
_diffrn_orient_matrix_UB_32      -0.0780025000
_diffrn_orient_matrix_UB_33      -0.3169615000
_diffrn_oxdiff_digest_frames     
;
01c9caf4ce7fd0aebbc3ee5afecc1b64f7004223069
;
_diffrn_oxdiff_digest_hkl        
;
019e8d02ca8a4cb40eed380ffa5e1875cbf828
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1035
_reflns_number_total             1166
_reflns_odcompleteness_completeness 83.16
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     50.38
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.102
_refine_diff_density_min         -0.971
_refine_diff_density_rms         0.226
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     131
_refine_ls_number_reflns         1166
_refine_ls_number_restraints     43
_refine_ls_R_factor_all          0.1249
_refine_ls_R_factor_gt           0.1192
_refine_ls_restrained_S_all      1.097
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1721P)²+64.5237P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3454
_refine_ls_wR_factor_ref         0.3489
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.602(9)
 0.398(9)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Restrained distances
 Re1-O4 = Re1-O1 = Re1-O2 = Re1-O3
 1.7 with sigma of 0.02
 O2-O1 \\sim O3-O4 \\sim O2-O3 \\sim O2-O4 \\sim O1-O3 \\sim O1-O4
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O4) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: Re1(0.25) O4(0.25) O2(0.25) O1(0.25) O3(0.25)
6.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C6(H6)
;


# start Validation Reply Form
_vrf_PLAT029_exp_1983            
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low      0.810      
RESPONSE: The cristal were small and twinned and out of 3 trials, 
this is the best dataset obtained despite a long exposure time
;
# end Validation Reply Form


_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re -0.0024(3) 0.3445(4) 0.5920(15) 0.085(2) Uani 0.25 1 d D . . A -1
S2 S 0.23295(11) 0.6205(3) 0.2496(10) 0.0315(10) Uani 1 1 d . . . . .
C4 C 0.2959(6) 0.500000 0.514(7) 0.032(5) Uani 1 2 d S T P . .
S3 S 0.32266(11) 0.6216(3) 0.6271(12) 0.0354(11) Uani 1 1 d . . . . .
C3 C 0.2596(6) 0.500000 0.359(7) 0.031(5) Uani 1 2 d S T P . .
C2 C 0.1910(4) 0.5537(12) 0.044(4) 0.028(3) Uani 1 1 d . . . . .
C1 C 0.1103(5) 0.5514(13) 0.004(5) 0.041(4) Uani 1 1 d . . . . .
H1 H 0.086940 0.587613 0.079289 0.050 Uiso 1 1 calc R . . . .
S4 S 0.40584(12) 0.6364(3) 0.9820(14) 0.0442(12) Uani 1 1 d . . . . .
C6 C 0.4464(5) 0.5536(17) 0.849(6) 0.053(5) Uani 1 1 d . . . . .
H6 H 0.469674 0.589889 0.771991 0.063 Uiso 1 1 calc R . . . .
O4 O 0.0471(6) 0.330(3) 0.535(12) 0.055(13) Uani 0.25 1 d D U . A -1
C5 C 0.3652(4) 0.5563(13) 0.820(5) 0.036(4) Uani 1 1 d . . . . .
O2 O -0.0298(13) 0.275(5) 0.269(11) 0.10(2) Uani 0.25 1 d D U . A -1
O1 O -0.0136(14) 0.287(4) 0.985(9) 0.10(2) Uani 0.25 1 d D U . A -1
S1 S 0.15083(12) 0.6346(3) -0.1272(12) 0.0377(11) Uani 1 1 d . . . . .
O3 O -0.0161(15) 0.478(2) 0.588(17) 0.19(6) Uani 0.25 1 d D U . A -1


_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
Re1 O4 1.679(19) . ?
Re1 O2 1.71(2) . ?
Re1 O1 1.72(2) . ?
Re1 O3 1.68(2) . ?
S2 C3 1.751(13) . ?
S2 C2 1.757(15) . ?
C4 S3 1.766(13) . ?
C4 S3 1.767(13) 6_565 ?
C4 C3 1.31(3) . ?
S3 C5 1.744(16) . ?
C2 C2 1.31(3) 6_565 ?
C2 S1 1.751(15) . ?
C1 C1 1.25(3) 6_565 ?
C1 S1 1.777(17) . ?
S4 C6 1.779(19) . ?
S4 C5 1.747(16) . ?
C6 C6 1.30(4) 6_565 ?
C5 C5 1.37(3) 6_565 ?

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
O4 Re1 O2 109.5(12) . . ?
O4 Re1 O1 109.5(12) . . ?
O4 Re1 O3 111.5(12) . . ?
O2 Re1 O1 107.6(11) . . ?
O3 Re1 O2 109.7(12) . . ?
O3 Re1 O1 109.0(12) . . ?
C3 S2 C2 95.4(8) . . ?
S3 C4 S3 113.9(13) . 6_565 ?
C3 C4 S3 123.0(7) . 6_565 ?
C3 C4 S3 123.0(7) . . ?
C5 S3 C4 95.9(8) . . ?
S2 C3 S2 113.9(13) 6_565 . ?
C4 C3 S2 123.0(7) . . ?
C4 C3 S2 123.0(7) . 6_565 ?
C2 C2 S2 117.6(5) 6_565 . ?
C2 C2 S1 124.2(5) 6_565 . ?
S1 C2 S2 118.1(8) . . ?
C1 C1 S1 124.7(5) 6_565 . ?
C5 S4 C6 99.3(8) . . ?
C6 C6 S4 124.5(7) 6_565 . ?
S3 C5 S4 118.9(9) . . ?
C5 C5 S3 117.1(5) 6_565 . ?
C5 C5 S4 123.9(5) 6_565 . ?
C2 S1 C1 98.3(7) . . ?



_ins_header                      
;
TITL exp_1983 in C2/m 
REM C2/m (#12 in standard setting)
CELL 1.54184  33.133475  12.173867   3.826283  90.0000  93.3600  90.0000
ZERR    4.00   0.003249   0.001447   0.000588   0.0000   0.0114   0.0000
LATT  7
SYMM -x, y,-z 
SFAC C H O S Re
UNIT 36.00 16.00 16.00 32.00 4.00
REM  CrysAlisPro recorded range (K): Min=199.9; max=200.1; aver:200.0
TEMP -73
SIZE 0.03 0.10 0.22
TREF
HKLF 4
END
;
_olex2_exptl_crystal_mounting_method 'paraffin oil'
_olex2_submission_original_sample_id exp_1983
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.267
_oxdiff_exptl_absorpt_empirical_full_min 0.487
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.602(9)
2 0.398(9)
####################################################################### 
# 
# 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_exp_1995_auto
_database_code_depnum_ccdc_archive 'CCDC 2296889'
loop_
_audit_author_name
_audit_author_address
'Narcis Avarvari'
;CNRS University of Angers
France
;
_audit_update_record             
;
2023-09-22 deposited with the CCDC.	2024-01-30 downloaded from the CCDC.
;
_audit_creation_date             2023-07-07
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
nicolas.zigon@univ-angers.fr
_chemical_name_common            ?
_chemical_name_systematic        'BVDTTTF I3'
_chemical_formula_moiety         '2(I0.6), C10 H4 S8'
_chemical_formula_sum            'C10 H4 I1.20 S8'
_chemical_formula_weight         532.89
_chemical_melting_point          ?
_chemical_oxdiff_formula         c40H10S32I6
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   3.777(19)
_cell_length_b                   12.18(14)
_cell_length_c                   33.1(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1523(44)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    29
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      61.9990
_cell_measurement_theta_min      12.8620
_shelx_estimated_absorpt_T_max   0.468
_shelx_estimated_absorpt_T_min   0.044
_exptl_absorpt_coefficient_mu    29.814
_exptl_absorpt_correction_T_max  0.583
_exptl_absorpt_correction_T_min  0.044
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.118a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    2.324
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1022
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -1 0 0.0467
0 1 0 0.0467
1 0 -2 0.1385
-1 0 2 0.1385
1 0 0 0.0133
-1 0 0 0.0133

_exptl_crystal_preparation       
'diffusion of I2 in a CHCl3 solution of BVDTTTF'
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.0141 -1.0005 -0.0010 -0.0928 0.0611 0.0595
0.0141 1.0005 0.0010 0.0928 -0.0611 -0.0595
0.8883 0.0025 -1.9990 -0.3253 0.2021 -0.7101
-0.8883 -0.0025 1.9990 0.3253 -0.2021 0.7101
1.0001 -0.0026 -0.0005 -0.0268 -0.0389 -0.0018
-1.0001 0.0026 0.0005 0.0268 0.0389 0.0018

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0592
_diffrn_reflns_av_unetI/netI     0.0561
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            3568
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.256
_diffrn_reflns_theta_min         2.670
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1990
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -16.00  29.00   1.00   22.15    --   42.94 -38.00 -90.00   45
  2  ω     -7.00  86.00   1.00   22.15    --   42.94   0.00  90.00   93
  3  ω     76.00 156.00   1.00   58.58    --  103.00  61.00-180.00   80
  4  ω     32.00  62.00   1.00   58.58    --  103.00 -77.00-120.00   30
  5  ω     61.00  87.00   1.00   58.58    --  103.00 -77.00 -90.00   26
  6  ω     92.00 132.00   1.00   58.58    --  103.00  77.00-150.00   40
  7  ω     82.00 153.00   1.00   58.58    --  103.00  77.00 -60.00   71
  8  ω     51.00 104.00   1.00   58.58    --  103.00 -77.00-180.00   53
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'SuperNova, Single source at offset/far, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0265205000
_diffrn_orient_matrix_UB_12      0.0929727000
_diffrn_orient_matrix_UB_13      0.1510711000
_diffrn_orient_matrix_UB_21      -0.0390958000
_diffrn_orient_matrix_UB_22      -0.0603787000
_diffrn_orient_matrix_UB_23      -0.1185319000
_diffrn_orient_matrix_UB_31      -0.0017708000
_diffrn_orient_matrix_UB_32      -0.0598429000
_diffrn_orient_matrix_UB_33      0.3543506000
_diffrn_oxdiff_digest_frames     
;
01731914cdee564831f364e4efd5bb652a004582605
;
_diffrn_oxdiff_digest_hkl        
;
01061966e46c92e33c0a94869a4025c788418c
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1207
_reflns_number_total             1518
_reflns_odcompleteness_completeness 98.36
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.261
_refine_diff_density_min         -0.755
_refine_diff_density_rms         0.226
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     103
_refine_ls_number_reflns         1518
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0943
_refine_ls_R_factor_gt           0.0795
_refine_ls_restrained_S_all      1.127
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1176P)²+20.0232P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2430
_refine_ls_wR_factor_ref         0.2540
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 C3, C4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Fixed Sof: I1(0.4) I2(0.2)
5.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C1(H1)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I -0.3242(11) 0.42274(18) 0.74303(7) 0.0551(7) Uani 0.4 1 d . . . A -1
I2 I 0.424(2) 0.4212(3) 0.74986(12) 0.0430(9) Uani 0.2 1 d . . . A -1
S2 S 0.7330(6) 0.62930(18) 0.48332(7) 0.0235(6) Uani 1 1 d . . . . .
S3 S 0.3956(6) 0.62925(18) 0.57383(7) 0.0246(6) Uani 1 1 d . . . . .
S1 S 1.0682(7) 0.6161(2) 0.39998(7) 0.0289(6) Uani 1 1 d . . . . .
S4 S 0.0773(7) 0.6148(2) 0.65797(7) 0.0311(6) Uani 1 1 d . . . . .
C4 C 0.495(3) 0.750000 0.5478(4) 0.021(2) Uani 1 2 d S TU P . .
C5 C 0.220(3) 0.6959(8) 0.6166(3) 0.0254(19) Uani 1 1 d . . . . .
C2 C 0.916(2) 0.6957(8) 0.4410(3) 0.0250(19) Uani 1 1 d . . . . .
C3 C 0.636(3) 0.750000 0.5096(4) 0.022(2) Uani 1 2 d S TU P . .
C6 C 0.233(3) 0.6970(9) 0.6985(3) 0.033(2) Uani 1 1 d . . . . .
H6 H 0.321804 0.660646 0.721726 0.039 Uiso 1 1 calc R . . . .
C1 C 0.911(3) 0.6959(9) 0.3590(3) 0.036(2) Uani 1 1 d . . . . .
H1 H 0.822023 0.658896 0.335844 0.044 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I1 I2 2.834(15) . ?
S2 C2 1.76(3) . ?
S2 C3 1.75(2) . ?
S3 C4 1.745(19) . ?
S3 C5 1.76(3) . ?
S1 C2 1.77(3) . ?
S1 C1 1.77(3) . ?
S4 C5 1.77(3) . ?
S4 C6 1.77(3) . ?
C4 C3 1.37(4) . ?
C5 C5 1.32(2) 7_575 ?
C2 C2 1.32(2) 7_575 ?
C6 C6 1.29(3) 7_575 ?
C1 C1 1.32(3) 7_575 ?

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
C3 S2 C2 95.3(13) . . ?
C4 S3 C5 95.1(13) . . ?
C2 S1 C1 100.3(16) . . ?
C5 S4 C6 99.7(16) . . ?
S3 C4 S3 114.9(15) 7_575 . ?
C3 C4 S3 122.6(7) . . ?
C3 C4 S3 122.6(7) . 7_575 ?
S3 C5 S4 118.6(14) . . ?
C5 C5 S3 117.4(6) 7_575 . ?
C5 C5 S4 123.9(7) 7_575 . ?
S2 C2 S1 119.2(13) . . ?
C2 C2 S2 117.4(6) 7_575 . ?
C2 C2 S1 123.3(7) 7_575 . ?
S2 C3 S2 114.6(15) 7_575 . ?
C4 C3 S2 122.7(7) . . ?
C4 C3 S2 122.7(7) . 7_575 ?
C6 C6 S4 124.4(7) 7_575 . ?
C1 C1 S1 123.3(7) 7_575 . ?



_ins_header                      
;
TITL exp_1995_auto in Pmmn 
REM Pmmn (#59, found as Pnmm in -cba setting)
CELL 1.54184  33.101873  12.178252   3.777463  90.0000  90.0000  90.0000
ZERR    1.00   0.852158   0.140735   0.019319   0.0000   0.0000   0.0000
LATT  1
SYMM -x+1/2,-y+1/2, z 
SYMM -x, y+1/2,-z 
SYMM  x+1/2,-y,-z 
SFAC C H S I
UNIT 40.00 10.00 32.00 6.00
REM  CrysAlisPro recorded range (K): Min=199.9; max=200.0; aver:200.0
TEMP -73
SIZE 0.03 0.09 0.28
TREF
HKLF 4
END
;
_olex2_exptl_crystal_mounting_method 'paraffin oil'
_olex2_submission_original_sample_id 'BVDTTTF I3'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.649
_oxdiff_exptl_absorpt_empirical_full_min 0.500
####################################################################### 
# 
# 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_exp_2007_auto
_database_code_depnum_ccdc_archive 'CCDC 2296891'
loop_
_audit_author_name
_audit_author_address
'Narcis Avarvari'
;CNRS University of Angers
France
;
_audit_update_record             
;
2023-09-22 deposited with the CCDC.	2024-01-30 downloaded from the CCDC.
;
_audit_creation_date             2023-07-07
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
nicolas.zigon@univ-angers.fr
_chemical_name_common            ?
_chemical_name_systematic        'EV-TTF ClO4'
_chemical_formula_moiety         'C10 H6 S8, C0.5 H Cl, Cl O4'
_chemical_formula_sum            'C10.50 H7 Cl2 O4 S8'
_chemical_formula_weight         524.54
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C10 S8 H6 Cl O4'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   8.0005(4)
_cell_length_b                   23.8718(10)
_cell_length_c                   9.8100(5)
_cell_angle_alpha                90
_cell_angle_beta                 100.649(5)
_cell_angle_gamma                90
_cell_volume                     1841.31(16)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3428
_cell_measurement_temperature    297.4(6)
_cell_measurement_theta_max      71.7350
_cell_measurement_theta_min      4.5440
_shelx_estimated_absorpt_T_max   0.423
_shelx_estimated_absorpt_T_min   0.086
_exptl_absorpt_coefficient_mu    11.819
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41785
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.118a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.892
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1056
_exptl_crystal_preparation       'electrocrystallization with TBAClO4'
_exptl_crystal_recrystallization_method 'electrocrystallization with TBAClO4'
_exptl_crystal_size_max          0.409
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.088
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_Laue_measured_fraction_full 0.946
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            6003
_diffrn_reflns_point_group_measured_fraction_full 0.946
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        66.587
_diffrn_reflns_theta_max         66.587
_diffrn_reflns_theta_min         3.703
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      297.4(6)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1990
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.946
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -25.00   7.00   1.00    5.08    --  -41.86  19.00  60.00   32
  2  ω    -22.00  36.00   1.00    5.08    --  -41.86  19.00   0.00   58
  3  ω    -38.00  -7.00   1.00    5.08    --   41.86 -19.00  30.00   31
  4  ω    -32.00  -3.00   1.00    5.08    --   41.86 -19.00 150.00   29
  5  ω    108.00 158.00   1.00   20.31    --  103.45  77.00  30.00   50
  6  ω     31.00  56.00   1.00   20.31    --  103.45 -61.00-120.00   25
  7  ω     96.00 150.00   1.00   20.31    --  103.45  77.00 -30.00   54
  8  ω    129.00 155.00   1.00   20.31    --  103.45  77.00 -90.00   26
  9  ω     79.00 105.00   1.00   20.31    --  103.45 -77.00  30.00   26
 10  ω     27.00 105.00   1.00   20.31    --  103.45 -77.00 -90.00   78
 11  ω     32.00  68.00   1.00   20.31    --  103.45 -61.00  90.00   36
 12  ω     78.00 153.00   1.00   20.31    --  103.45  45.00  30.00   75
 13  ω    105.00 157.00   1.00   20.31    --  103.45  77.00 -60.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'SuperNova, Single source at offset/far, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1279471000
_diffrn_orient_matrix_UB_12      -0.0471436000
_diffrn_orient_matrix_UB_13      -0.0120537000
_diffrn_orient_matrix_UB_21      -0.0258919000
_diffrn_orient_matrix_UB_22      0.0096777000
_diffrn_orient_matrix_UB_23      -0.1578688000
_diffrn_orient_matrix_UB_31      0.1460378000
_diffrn_orient_matrix_UB_32      0.0429701000
_diffrn_orient_matrix_UB_33      0.0222010000
_diffrn_oxdiff_digest_frames     
;
018ca4ab4e0dfae2443241ccd1a5824aa1000281ff2
;
_diffrn_oxdiff_digest_hkl        
;
014ade43d5aa3dbec0b09cfcdfe91078c29c66
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2614
_reflns_number_total             3084
_reflns_odcompleteness_completeness 94.14
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.984
_refine_diff_density_min         -0.938
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         3084
_refine_ls_number_restraints     186
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0570
_refine_ls_restrained_S_all      1.120
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0951P)²+1.9994P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1564
_refine_ls_wR_factor_ref         0.1653
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Shared sites
{Cl2, Cl3}
3. Restrained distances
 O3-O5 \\sim O4-O6 \\sim O3-O6 \\sim O4-O5 \\sim O3-O4 \\sim O5-O6
 with sigma of 0.04
 Cl3-O1 \\sim Cl3-O2 \\sim Cl3-O7 \\sim Cl3-O8
 with sigma of 0.02
 O1-O7 \\sim O2-O8 \\sim O1-O8 \\sim O2-O7 \\sim O1-O2 \\sim O7-O8
 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
O3 \\sim O4 \\sim O5 \\sim O6: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
Cl3 \\sim O1 \\sim O2 \\sim O7 \\sim O8: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(O3) \\sim Ueq, Uanis(Cl2) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O5) \\sim
Ueq, Uanis(O6) \\sim Ueq, Uanis(Cl3) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O2)
\\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O8) \\sim Ueq: with sigma of 0.05 and
sigma for terminal atoms of 0.1
Uanis(C1) \\sim Ueq, Uanis(Cl1) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(Cl2) = Uanis(Cl3)
5. Rigid body (RIGU) restrains
 O3, O4, O5, O6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl3, O1, O2, O7, O8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O3, Cl2, O4, O5, O6, Cl3, O1, O2, O7, O8
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C1, Cl1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: C1(0.5) H1A(0.5) H1B(0.5) O3(0.5) Cl2(0.5) O4(0.5) O5(0.5) O6(0.5)
 Cl3(0.5) O1(0.5) O2(0.5) O7(0.5) O8(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C00J(H00A,H00B), C00K(H00C,H00D)
7.b Aromatic/amide H refined with riding coordinates:
 C00H(H00H), C00I(H00I)
;


_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S001 S 0.70068(13) 0.52737(4) 0.42603(11) 0.0408(3) Uani 1 1 d . . . . .
C1 C 0.566(3) 0.4649(6) 1.0444(18) 0.136(9) Uani 0.5 1 d . U P . .
H1A H 0.659151 0.465175 1.123087 0.163 Uiso 0.5 1 calc R . P . .
H1B H 0.538115 0.426296 1.018953 0.163 Uiso 0.5 1 calc R . P . .
Cl1 Cl 0.6216(3) 0.49926(13) 0.9102(3) 0.1276(9) Uani 1 1 d . U . . .
S002 S 0.75514(13) 0.41387(4) 0.61428(11) 0.0422(3) Uani 1 1 d . . . . .
S003 S 1.00750(14) 0.47338(4) 0.81621(11) 0.0431(3) Uani 1 1 d . . . . .
S004 S 0.95888(15) 0.58249(4) 0.63032(12) 0.0464(3) Uani 1 1 d . . . . .
S005 S 0.79930(16) 0.30602(4) 0.77458(13) 0.0501(3) Uani 1 1 d . . . . .
S006 S 0.62285(15) 0.62502(5) 0.24498(14) 0.0526(3) Uani 1 1 d . . . . .
S007 S 1.07525(18) 0.37513(5) 1.00744(13) 0.0559(3) Uani 1 1 d . . . . .
S008 S 0.93023(18) 0.69221(5) 0.49460(15) 0.0565(4) Uani 1 1 d . . . . .
C00B C 0.8563(5) 0.37585(17) 0.7558(5) 0.0402(9) Uani 1 1 d . . . . .
C00C C 0.8634(6) 0.62317(17) 0.4929(5) 0.0406(9) Uani 1 1 d . . . . .
C00D C 0.7420(5) 0.59747(17) 0.3959(5) 0.0389(9) Uani 1 1 d . . . . .
C00E C 0.8471(5) 0.52253(17) 0.5791(5) 0.0391(9) Uani 1 1 d . . . . .
C00F C 0.8678(5) 0.47454(17) 0.6592(4) 0.0379(9) Uani 1 1 d . . . . .
C00G C 0.9722(5) 0.40368(18) 0.8512(5) 0.0414(9) Uani 1 1 d . . . . .
C00H C 0.9071(8) 0.3341(2) 1.0464(6) 0.0645(15) Uani 1 1 d . . . . .
H00H H 0.894604 0.331831 1.138625 0.077 Uiso 1 1 calc R . . . .
C00I C 0.7974(8) 0.3063(2) 0.9532(6) 0.0598(13) Uani 1 1 d . . . . .
H00I H 0.713653 0.285540 0.984392 0.072 Uiso 1 1 calc R . . . .
C00J C 0.6995(8) 0.6961(2) 0.2471(7) 0.0670(15) Uani 1 1 d . . . . .
H00A H 0.799671 0.696935 0.204586 0.080 Uiso 1 1 calc R . . . .
H00B H 0.613114 0.719065 0.190884 0.080 Uiso 1 1 calc R . . . .
C00K C 0.7433(9) 0.7214(2) 0.3883(8) 0.0758(18) Uani 1 1 d . . . . .
H00C H 0.647814 0.716497 0.435335 0.091 Uiso 1 1 calc R . . . .
H00D H 0.760373 0.761375 0.378732 0.091 Uiso 1 1 calc R . . . .
O3 O 0.529(2) 0.6644(7) 0.8493(16) 0.122(5) Uani 0.5 1 d D U P A 1
Cl2 Cl 0.4654(2) 0.65421(6) 0.70741(18) 0.0708(4) Uani 0.5 1 d . U P A 1
O4 O 0.2902(15) 0.6623(8) 0.6874(15) 0.143(5) Uani 0.5 1 d D U P A 1
O5 O 0.504(2) 0.5981(5) 0.6715(14) 0.104(4) Uani 0.5 1 d D U P A 1
O6 O 0.516(3) 0.6882(8) 0.613(2) 0.195(9) Uani 0.5 1 d D U P A 1
Cl3 Cl 0.4654(2) 0.65421(6) 0.70741(18) 0.0708(4) Uani 0.5 1 d D U P B 2
O1 O 0.4041(18) 0.6872(7) 0.5879(18) 0.133(5) Uani 0.5 1 d D U P B 2
O2 O 0.452(3) 0.6836(9) 0.8296(18) 0.170(7) Uani 0.5 1 d D U P B 2
O7 O 0.6439(13) 0.6591(6) 0.7100(13) 0.111(3) Uani 0.5 1 d D U P B 2
O8 O 0.392(3) 0.6030(6) 0.7044(16) 0.161(8) Uani 0.5 1 d D U P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S001 C00D 1.742(4) . ?
S001 C00E 1.729(5) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 Cl1 1.85(3) 3_667 ?
C1 Cl1 1.68(2) . ?
S002 C00B 1.729(4) . ?
S002 C00F 1.719(4) . ?
S003 C00F 1.728(4) . ?
S003 C00G 1.732(4) . ?
S004 C00C 1.722(5) . ?
S004 C00E 1.713(4) . ?
S005 C00B 1.747(4) . ?
S005 C00I 1.755(6) . ?
S006 C00D 1.735(5) . ?
S006 C00J 1.803(5) . ?
S007 C00G 1.740(5) . ?
S007 C00H 1.762(6) . ?
S008 C00C 1.732(4) . ?
S008 C00K 1.798(7) . ?
C00B C00G 1.362(6) . ?
C00C C00D 1.372(6) . ?
C00E C00F 1.382(6) . ?
C00H H00H 0.9300 . ?
C00H C00I 1.323(8) . ?
C00I H00I 0.9300 . ?
C00J H00A 0.9700 . ?
C00J H00B 0.9700 . ?
C00J C00K 1.493(9) . ?
C00K H00C 0.9700 . ?
C00K H00D 0.9700 . ?
O3 Cl2 1.412(13) . ?
Cl2 O4 1.392(11) . ?
Cl2 O5 1.433(11) . ?
Cl2 O6 1.351(14) . ?
Cl3 O1 1.422(11) . ?
Cl3 O2 1.411(11) . ?
Cl3 O7 1.428(10) . ?
Cl3 O8 1.353(10) . ?

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
C00E S001 C00D 95.3(2) . . ?
H1A C1 H1B 108.4 . . ?
Cl1 C1 H1A 110.1 . . ?
Cl1 C1 H1A 110.1 3_667 . ?
Cl1 C1 H1B 110.1 . . ?
Cl1 C1 H1B 110.1 3_667 . ?
Cl1 C1 Cl1 107.9(9) . 3_667 ?
C1 Cl1 C1 72.1(9) . 3_667 ?
C00F S002 C00B 95.2(2) . . ?
C00F S003 C00G 95.1(2) . . ?
C00E S004 C00C 96.3(2) . . ?
C00B S005 C00I 98.7(2) . . ?
C00D S006 C00J 102.4(2) . . ?
C00G S007 C00H 98.7(3) . . ?
C00C S008 C00K 98.1(3) . . ?
S002 C00B S005 119.5(3) . . ?
C00G C00B S002 117.0(3) . . ?
C00G C00B S005 123.4(3) . . ?
S004 C00C S008 116.0(3) . . ?
C00D C00C S004 116.5(3) . . ?
C00D C00C S008 127.6(4) . . ?
S006 C00D S001 114.7(2) . . ?
C00C C00D S001 116.4(3) . . ?
C00C C00D S006 129.0(3) . . ?
S004 C00E S001 115.6(2) . . ?
C00F C00E S001 122.7(3) . . ?
C00F C00E S004 121.7(3) . . ?
S002 C00F S003 115.9(2) . . ?
C00E C00F S002 123.4(3) . . ?
C00E C00F S003 120.6(3) . . ?
S003 C00G S007 118.8(3) . . ?
C00B C00G S003 116.6(3) . . ?
C00B C00G S007 124.5(3) . . ?
S007 C00H H00H 117.8 . . ?
C00I C00H S007 124.3(4) . . ?
C00I C00H H00H 117.8 . . ?
S005 C00I H00I 117.8 . . ?
C00H C00I S005 124.4(4) . . ?
C00H C00I H00I 117.8 . . ?
S006 C00J H00A 108.7 . . ?
S006 C00J H00B 108.7 . . ?
H00A C00J H00B 107.6 . . ?
C00K C00J S006 114.4(4) . . ?
C00K C00J H00A 108.7 . . ?
C00K C00J H00B 108.7 . . ?
S008 C00K H00C 108.7 . . ?
S008 C00K H00D 108.7 . . ?
C00J C00K S008 114.1(4) . . ?
C00J C00K H00C 108.7 . . ?
C00J C00K H00D 108.7 . . ?
H00C C00K H00D 107.6 . . ?
O3 Cl2 O5 110.4(8) . . ?
O4 Cl2 O3 106.6(9) . . ?
O4 Cl2 O5 110.7(9) . . ?
O6 Cl2 O3 118.4(12) . . ?
O6 Cl2 O4 104.1(11) . . ?
O6 Cl2 O5 106.6(10) . . ?
O1 Cl3 O7 99.2(8) . . ?
O2 Cl3 O1 110.8(12) . . ?
O2 Cl3 O7 100.3(9) . . ?
O8 Cl3 O1 113.6(9) . . ?
O8 Cl3 O2 111.5(11) . . ?
O8 Cl3 O7 120.1(11) . . ?

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
S001 C00E C00F S002 1.7(6) . . . . ?
S001 C00E C00F S003 -176.3(2) . . . . ?
Cl1 C1 Cl1 C1 0.001(2) 3_667 . . 3_667 ?
S002 C00B C00G S003 -1.6(5) . . . . ?
S002 C00B C00G S007 174.5(2) . . . . ?
S004 C00C C00D S001 0.4(5) . . . . ?
S004 C00C C00D S006 -179.3(3) . . . . ?
S004 C00E C00F S002 178.4(2) . . . . ?
S004 C00E C00F S003 0.4(5) . . . . ?
S005 C00B C00G S003 -178.3(2) . . . . ?
S005 C00B C00G S007 -2.1(6) . . . . ?
S006 C00J C00K S008 70.1(6) . . . . ?
S007 C00H C00I S005 -0.6(8) . . . . ?
S008 C00C C00D S001 -178.7(3) . . . . ?
S008 C00C C00D S006 1.6(7) . . . . ?
C00B S002 C00F S003 -4.2(3) . . . . ?
C00B S002 C00F C00E 177.7(4) . . . . ?
C00B S005 C00I C00H -37.8(5) . . . . ?
C00C S004 C00E S001 0.2(3) . . . . ?
C00C S004 C00E C00F -176.7(4) . . . . ?
C00C S008 C00K C00J -58.6(5) . . . . ?
C00D S001 C00E S004 0.0(3) . . . . ?
C00D S001 C00E C00F 176.8(4) . . . . ?
C00D S006 C00J C00K -35.4(5) . . . . ?
C00E S001 C00D S006 179.5(2) . . . . ?
C00E S001 C00D C00C -0.2(4) . . . . ?
C00E S004 C00C S008 178.9(3) . . . . ?
C00E S004 C00C C00D -0.4(4) . . . . ?
C00F S002 C00B S005 -179.7(3) . . . . ?
C00F S002 C00B C00G 3.5(4) . . . . ?
C00F S003 C00G S007 -177.5(3) . . . . ?
C00F S003 C00G C00B -1.2(4) . . . . ?
C00G S003 C00F S002 3.6(3) . . . . ?
C00G S003 C00F C00E -178.3(4) . . . . ?
C00G S007 C00H C00I 37.8(6) . . . . ?
C00H S007 C00G S003 139.9(3) . . . . ?
C00H S007 C00G C00B -36.2(4) . . . . ?
C00I S005 C00B S002 -137.6(3) . . . . ?
C00I S005 C00B C00G 39.0(4) . . . . ?
C00J S006 C00D S001 -179.4(3) . . . . ?
C00J S006 C00D C00C 0.3(5) . . . . ?
C00K S008 C00C S004 -155.8(3) . . . . ?
C00K S008 C00C C00D 23.3(5) . . . . ?


_olex2_exptl_crystal_mounting_method 'paraffin oil'
_olex2_submission_original_sample_id exp_2007
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.125
_oxdiff_exptl_absorpt_empirical_full_min 0.389
