# Supplementary Material (ESI) for Journal of Materials Chemistry
# This journal is © The Royal Society of Chemistry 2000
# CCDC Number: 1145/217

data_global

_publ_contact_author               'Andrei S.Batsanov'
_publ_contact_author_email          a.s.batsanov@durham.ac.uk

loop_
_publ_author_name
 'John, Derek E.'
 'Moore, Adrian J.'
 'Bryce, Martin R.'
 'Batsanov, Andrei S.'
 'Leech, Michael A.' 
 'Howard, Judith A. K.' 
_journal_name_full              'Journal of Materials Chemistry'
_journal_volume                    '?'
_journal_page_first                '?'
_journal_page_last                 '?'
_journal_year                      '2000'
_ccdc_journal_depnumber            '?'

_publ_section_title
; New bis(tetrathiafulvalenyl) derivatives and their radical salts:
 synthetic and X-ray structural studies.
;

#======================================================END 
data_9
  
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
 4-bis[4',5,5'-tris(methylsulfanyl)tetrathiafulvalenyl] 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C18 H18 S14' 
_chemical_formula_weight          683.16 
_chemical_melting_point           '160-161 deg.C' 
_chemical_compound_source         ? 
  
_ccdc_compound_id                  '9'
_ccdc_biological_activity          '?'
_ccdc_polymorph                    '?'
_ccdc_disorder                     
; S(5), C(8), H(81,82,83) are disordered between two positions,
 A and B, with the occupancies 61.2(1) and 38.8(1)%.
;
_ccdc_comments                     '?'

loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0033   0.0016 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'S'  'S'   0.1246   0.1234 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
  
_symmetry_cell_setting            Monoclinic 
_symmetry_space_group_name_H-M    'P 1 21/n 1' 
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x-1/2, -y-1/2, z-1/2' 
  
_cell_length_a                    8.374(1) 
_cell_length_b                    12.684(2) 
_cell_length_c                    26.295(3) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  96.20(1) 
_cell_angle_gamma                 90.00 
_cell_volume                      2776.6(6) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     120(2) 
_cell_measurement_reflns_used     371 
_cell_measurement_theta_min       15.7 
_cell_measurement_theta_max       24.5 
  
_exptl_crystal_description        block 
_exptl_crystal_colour             red-brown 
_exptl_crystal_size_max           0.5 
_exptl_crystal_size_mid           0.4 
_exptl_crystal_size_min           0.2 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.634 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              1400 
_exptl_absorpt_coefficient_mu     1.104 
_exptl_absorpt_correction_type    multiscan 
_exptl_absorpt_correction_T_min   0.4647 
_exptl_absorpt_correction_T_max   0.6938 
_exptl_absorp_process_details
 'SADABS (G.M.Sheldrick,1997), R(int)=0.050 before correction' 
  
_exptl_special_details 
; 
The data collection nominally covered full sphere 
of reciprocal space, by a combination of 5 sets of exposures;
each set had a different \f and/or 2\q angles and each
exposure covered 0.3\% in \w. Crystal decay was monitored 
by repeating 50 initial frames at the end of 
data collection and comparing 360 duplicate reflections.
Crystal to detector distance 4.51 cm.
; 
  
_diffrn_ambient_temperature       120(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device        'SMART 1K CCD area detector' 
_diffrn_measurement_method        '\w scans' 
_diffrn_standards_number          'not measured' 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         0.14 
_diffrn_reflns_number             21201 
_diffrn_reflns_av_R_equivalents   0.0000 
_diffrn_reflns_av_sigmaI/netI     0.0470 
_diffrn_reflns_limit_h_min        -9 
_diffrn_reflns_limit_h_max        9 
_diffrn_reflns_limit_k_min        -15 
_diffrn_reflns_limit_k_max        15 
_diffrn_reflns_limit_l_min        -31 
_diffrn_reflns_limit_l_max        30 
_diffrn_reflns_theta_min          1.78 
_diffrn_reflns_theta_max          26.16 
_reflns_number_total              21201 
_reflns_number_observed           19392 
_reflns_observed_criterion        >2sigma(I) 
  
_computing_data_collection        SMART 
_computing_cell_refinement        SMART 
_computing_data_reduction         SAINT 
_computing_structure_solution     'SHELXS-86 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)' 
_computing_molecular_graphics     SHELXTL 
_computing_publication_material   SHELXTL 
  
_refine_special_details 
; 
 Refinement on F^2^ for ALL reflections except for 33 with very negative 
F^2^ 
 or flagged by the user for potential systematic errors.  Weighted R-
factors 
 wR and all goodnesses of fit S are based on F^2^, conventional R-
factors R 
 are based on F, with F set to zero for negative F^2^. The observed 
criterion 
 of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. 
and is 
 not relevant to the choice of reflections for refinement.
    Twinned crystal with the twin law h'=h, k'=-k, l'=-l-2h/3 
(reflections
 with |h|=3n almost perfectly overlap), the .HKL file was rewritten in 
 HKLF 5 format and the component contributions were refined to 66.10(7) 
 and 13.90(7)%. Without twin correction, R1(obs)=0.073, max. residual 
 electron density 1.03.  Laue equivalents were not merged due to the 
twin 
 correction. Actually, 5026 reflections are unique (R~int~=0.0317), 
 of which 4639 observed.  
    Methyl groups were refined as rigid bodies with a common (refined)
 U for three H atoms.
; 
  
_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme 
 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+10.3475P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     constr 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          21168 
_refine_ls_number_parameters      309 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0465 
_refine_ls_R_factor_obs           0.0420 
_refine_ls_wR_factor_all          0.1194 
_refine_ls_wR_factor_obs          0.1145 
_refine_ls_goodness_of_fit_all    1.187 
_refine_ls_goodness_of_fit_obs    1.203 
_refine_ls_restrained_S_all       1.199 
_refine_ls_restrained_S_obs       1.203 
_refine_ls_shift/esd_max          0.001 
_refine_ls_shift/esd_mean         0.000 
  
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_thermal_displace_type 
 _atom_site_occupancy 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_group 
S1 S 0.07372(7) 0.53391(5) 0.16303(3) 0.0308(2) Uani 1 d . . 
S2 S 0.31402(7) 0.37867(4) 0.13466(2) 0.02396(13) Uani 1 d . . 
S3 S -0.08302(8) 0.36809(5) 0.23130(3) 0.0352(2) Uani 1 d . . 
S4 S 0.14828(7) 0.20338(4) 0.20756(2) 0.02326(13) Uani 1 d . . 
S5A S -0.31517(13) 0.20529(8) 0.26862(4) 0.0279(2) Uani 0.6121(11) d P 1 
S5B S -0.2461(2) 0.23034(13) 0.30158(7) 0.0279(2) Uani 0.3879(11) d P 2 
S6 S -0.02445(10) 0.03286(5) 0.26116(3) 0.0520(2) Uani 1 d . . 
S7 S 0.44643(9) 0.53314(5) 0.06139(3) 0.0427(2) Uani 1 d . . 
S11 S 0.28771(7) 0.78610(4) 0.14228(2) 0.02350(13) Uani 1 d . . 
S12 S 0.07805(7) 0.85353(4) 0.05037(2) 0.02311(13) Uani 1 d . . 
S13 S 0.46816(7) 1.01991(4) 0.14333(2) 0.02414(13) Uani 1 d . . 
S14 S 0.25810(7) 1.07714(4) 0.05032(2) 0.02486(13) Uani 1 d . . 
S15 S 0.72838(7) 1.17238(5) 0.12212(2) 0.02893(14) Uani 1 d . . 
S16 S 0.48861(8) 1.24097(5) 0.01730(2) 0.03109(15) Uani 1 d . . 
S17 S -0.02572(7) 0.63149(5) 0.02212(2) 0.02998(14) Uani 1 d . . 
C1 C 0.1491(3) 0.4043(2) 0.16903(8) 0.0198(5) Uani 1 d . . 
C2 C 0.2103(3) 0.5765(2) 0.12122(8) 0.0207(5) Uani 1 d . . 
C3 C 0.3180(3) 0.5062(2) 0.10781(9) 0.0241(5) Uani 1 d . . 
C4 C 0.0802(3) 0.3338(2) 0.19800(8) 0.0194(5) Uani 1 d . . 
C5 C -0.1172(3) 0.2379(2) 0.25112(11) 0.0420(7) Uani 1 d . . 
C6 C -0.0119(3) 0.1639(2) 0.24106(9) 0.0278(5) Uani 1 d . . 
C7 C 0.6367(3) 0.4890(2) 0.09281(14) 0.0558(9) Uani 1 d . . 
H71 H 0.7227(4) 0.5096(12) 0.0723(3) 0.053(5) Uiso 1 d R . 
H72 H 0.6353(8) 0.4120(3) 0.0962(6) 0.053(5) Uiso 1 d R . 
H73 H 0.6560(10) 0.5211(10) 0.1268(3) 0.053(5) Uiso 1 d R . 
C8A C -0.2848(6) 0.2612(4) 0.3320(2) 0.0442(12) Uani 0.6121(11) d P 1 
H81A H -0.3865(10) 0.2598(22) 0.3475(5) 0.066 Uiso 0.6121(11) d PR 1 
H82A H -0.2484(34) 0.3345(8) 0.3298(2) 0.066 Uiso 0.6121(11) d PR 1 
H83A H -0.2037(26) 0.2206(14) 0.3535(4) 0.066 Uiso 0.6121(11) d PR 1 
C8B C -0.4192(9) 0.2158(5) 0.2537(3) 0.035(2) Uiso 0.3879(11) d P 2 
H81B H -0.5169(9) 0.2097(5) 0.2710(3) 0.053 Uiso 0.3879(11) d PR 2 
H82B H -0.4066(9) 0.1524(5) 0.2333(3) 0.053 Uiso 0.3879(11) d PR 2 
H83B H -0.4274(9) 0.2778(5) 0.2313(3) 0.053 Uiso 0.3879(11) d PR 2 
C9 C 0.1083(3) -0.0347(2) 0.22336(9) 0.0375(6) Uani 1 d . . 
H91 H 0.1106(15) -0.1098(3) 0.2322(4) 0.044(4) Uiso 1 d R . 
H92 H 0.2169(5) -0.0055(8) 0.2298(4) 0.044(4) Uiso 1 d R . 
H93 H 0.0692(11) -0.0262(10) 0.18711(10) 0.044(4) Uiso 1 d R . 
C11 C 0.2358(2) 0.8870(2) 0.09720(8) 0.0198(5) Uani 1 d . . 
C12 C 0.1914(3) 0.6860(2) 0.10307(8) 0.0195(5) Uani 1 d . . 
C13 C 0.0959(3) 0.7168(2) 0.06169(8) 0.0208(5) Uani 1 d . . 
C14 C 0.3097(3) 0.9812(2) 0.09791(8) 0.0189(5) Uani 1 d .. . 
C15 C 0.5409(3) 1.1159(2) 0.10266(8) 0.0206(5) Uani 1 d . . 
C16 C 0.4454(3) 1.1414(2) 0.06008(8) 0.0211(5) Uani 1 d . . 
C17 C 0.0327(3) 0.6658(2) -0.04008(9) 0.0334(6) Uani 1 d . . 
H171 H -0.0244(15) 0.7300(7) -0.0523(3) 0.053(5) Uiso 1 d R . 
H172 H 0.0045(18) 0.6081(6) -0.0642(2) 0.053(5) Uiso 1 d R . 
H173 H 0.1488(4) 0.6783(13) -0.03754(15) 0.053(5) Uiso 1 d R . 
C18 C 0.8562(3) 1.0706(2) 0.10101(11) 0.0391(7) Uani 1 d . . 
H181 H 0.9690(3) 1.0886(6) 0.1112(5) 0.045(4) Uiso 1 d R . 
H182 H 0.8380(14) 1.0650(8) 0.06362(12) 0.045(4) Uiso 1 d R . 
H183 H 0.8314(13) 1.0028(3) 0.1163(5) 0.045(4) Uiso 1 d R . 
C19 C 0.4048(3) 1.1873(2) -0.04313(9) 0.0329(6) Uani 1 d . . 
H191 H 0.4388(16) 1.2300(8) -0.07140(9) 0.053(5) Uiso 1 d R . 
H192 H 0.2863(3) 1.1870(12) -0.0455(3) 0.053(5) Uiso 1 d R . 
H193 H 0.4429(16) 1.1143(5) -0.0465(3) 0.053(5) Uiso 1 d R . 
  
loop_ 
 _atom_site_aniso_label 
 _atom_site_aniso_U_11 
 _atom_site_aniso_U_22 
 _atom_site_aniso_U_33 
 _atom_site_aniso_U_23 
 _atom_site_aniso_U_13 
 _atom_site_aniso_U_12 
S1 0.0325(3) 0.0186(3) 0.0461(4) 0.0089(3) 0.0265(3) 0.0069(2) 
S2 0.0265(3) 0.0149(3) 0.0335(3) 0.0038(2) 0.0174(3) 0.0025(2) 
S3 0.0423(4) 0.0222(3) 0.0471(4) 0.0086(3) 0.0324(3) 0.0070(3) 
S4 0.0257(3) 0.0171(3) 0.0292(3) 0.0025(2) 0.0130(3) 0.0004(2) 
S5A 0.0263(5) 0.0329(5) 0.0267(5) -0.0010(4) 0.0126(4) -0.0088(4) 
S5B 0.0263(5) 0.0329(5) 0.0267(5) -0.0010(4) 0.0126(4) -0.0088(4) 
S6 0.0612(5) 0.0262(4) 0.0764(6) 0.0227(4) 0.0433(4) 0.0091(3) 
S7 0.0540(4) 0.0227(3) 0.0600(5) 0.0112(3) 0.0457(4) 0.0076(3) 
S11 0.0316(3) 0.0171(3) 0.0222(3) 0.0028(2) 0.0046(3) -0.0024(2) 
S12 0.0222(3) 0.0147(3) 0.0322(3) 0.0029(2) 0.0016(3) -0.0007(2) 
S13 0.0298(3) 0.0221(3) 0.0209(3) 0.0009(2) 0.0046(3) -0.0061(2) 
S14 0.0189(3) 0.0192(3) 0.0362(3) 0.0072(2) 0.0015(3) -0.0016(2) 
S15 0.0287(3) 0.0271(3) 0.0304(3) -0.0027(3) 0.0001(3) -0.0108(3) 
S16 0.0386(3) 0.0211(3) 0.0324(3) 0.0091(3) -0.0013(3) -0.0112(3) 
S17 0.0345(3) 0.0223(3) 0.0334(3) -0.0005(3) 0.0048(3) -0.0115(3) 
C1 0.0217(11) 0.0175(11) 0.0218(11) -0.0005(9) 0.0094(10) 0.0009(9) 
C2 0.0249(11) 0.0150(11) 0.0240(11) 0.0025(9) 0.0107(10) -0.0019(9) 
C3 0.0308(13) 0.0139(11) 0.0300(12) 0.0022(9) 0.0140(11) 0.0007(9) 
C4 0.0236(11) 0.0168(11) 0.0191(11) -0.0022(9) 0.0075(9) -0.0003(9) 
C5 0.046(2) 0.0271(14) 0.060(2) 0.0197(13) 0.0361(15) 0.0072(12) 
C6 0.0323(13) 0.0229(13) 0.0301(13) 0.0094(10) 0.0117(11) -0.0011(10) 
C7 0.034(2) 0.045(2) 0.095(3) -0.009(2) 0.041(2) -0.0063(13) 
C8A 0.050(3) 0.042(3) 0.045(3) -0.019(2) 0.026(2) -0.008(2) 
C9 0.059(2) 0.0250(14) 0.0292(14) 0.0065(11) 0.0058(13) 0.0083(13) 
C11 0.0201(11) 0.0187(11) 0.0215(11) -0.0018(9) 0.0068(9) 0.0017(9) 
C12 0.0229(11) 0.0131(11) 0.0243(11) -0.0013(9) 0.0108(10) 0.0007(9) 
C13 0.0222(11) 0.0148(11) 0.0268(12) -0.0004(9) 0.0094(10) -0.0016(9) 
C14 0.0206(11) 0.0178(11) 0.0195(11) -0.0009(9) 0.0068(9) 0.0014(9) 
C15 0.0246(12) 0.0158(11) 0.0222(11) -0.0027(9) 0.0055(10) -0.0031(9) 
C16 0.0220(11) 0.0135(11) 0.0292(12) -0.0010(9) 0.0099(10) -0.0020(9) 
C17 0.0423(15) 0.0268(14) 0.0310(13) -0.0032(11) 0.0026(12) -0.0023(11) 
C18 0.0225(13) 0.046(2) 0.047(2) 0.0044(13) 0.0003(12) -0.0006(12) 
C19 0.0400(15) 0.0341(14) 0.0264(13) 0.0013(11) 0.0123(12) -0.0057(12) 
  
_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 C2 1.755(2) . ? 
S1 C1 1.762(2) . ? 
S2 C1 1.760(2) . ? 
S2 C3 1.766(2) . ? 
S3 C4 1.756(2) . ? 
S3 C5 1.765(2) . ? 
S4 C6 1.756(2) . ? 
S4 C4 1.758(2) . ? 
S5A C8A 1.804(4) . ? 
S5A C5 1.815(3) . ? 
S5B C5 1.801(3) . ? 
S5B C8B 1.823(7) . ? 
S6 C6 1.750(2) . ? 
S6 C9 1.788(3) . ? 
S7 C3 1.746(2) . ? 
S7 C7 1.803(3) . ? 
S11 C11 1.767(2) . ? 
S11 C12 1.773(2) . ? 
S12 C11 1.758(2) . ? 
S12 C13 1.764(2) . ? 
S13 C14 1.757(2) . ? 
S13 C15 1.771(2) . ? 
S14 C16 1.761(2) . ? 
S14 C14 1.765(2) . ? 
S15 C15 1.751(2) . ? 
S15 C18 1.802(3) . ? 
S16 C16 1.755(2) . ? 
S16 C19 1.800(2) . ? 
S17 C13 1.749(2) . ? 
S17 C17 1.810(2) . ? 
C1 C4 1.345(3) . ? 
C2 C3 1.342(3) . ? 
C2 C12 1.472(3) . ? 
C5 C6 1.334(3) . ? 
C11 C14 1.345(3) . ? 
C12 C13 1.337(3) . ? 
C15 C16 1.343(3) . ? 
  
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
C2 S1 C1 95.27(10) . . ? 
C1 S2 C3 94.92(10) . . ? 
C4 S3 C5 94.31(11) . . ? 
C6 S4 C4 94.97(10) . . ? 
C8A S5A C5 95.9(2) . . ? 
C5 S5B C8B 89.5(2) . . ? 
C6 S6 C9 103.08(11) . . ? 
C3 S7 C7 101.52(13) . . ? 
C11 S11 C12 93.73(10) . . ? 
C11 S12 C13 94.36(10) . . ? 
C14 S13 C15 93.74(10) . . ? 
C16 S14 C14 94.00(10) . . ? 
C15 S15 C18 99.22(11) . . ? 
C16 S16 C19 101.88(11) . . ? 
C13 S17 C17 101.08(11) . . ? 
C4 C1 S2 125.2(2) . . ? 
C4 C1 S1 120.0(2) . . ? 
S2 C1 S1 114.82(11) . . ? 
C3 C2 C12 126.4(2) . . ? 
C3 C2 S1 117.5(2) . . ? 
C12 C2 S1 116.04(15) . . ? 
C2 C3 S7 122.4(2) . . ? 
C2 C3 S2 117.5(2) . . ? 
S7 C3 S2 119.89(12) . . ? 
C1 C4 S3 121.5(2) . . ? 
C1 C4 S4 123.7(2) . . ? 
S3 C4 S4 114.82(12) . . ? 
C6 C5 S3 117.9(2) . . ? 
C6 C5 S5B 124.8(2) . . ? 
S3 C5 S5B 113.35(15) . . ? 
C6 C5 S5A 122.1(2) . . ? 
S3 C5 S5A 118.01(14) . . ? 
C5 C6 S6 123.1(2) . . ? 
C5 C6 S4 117.1(2) . . ? 
S6 C6 S4 119.76(14) . . ? 
C14 C11 S12 122.3(2) . . ? 
C14 C11 S11 123.7(2) . . ? 
S12 C11 S11 114.00(12) . . ? 
C13 C12 C2 125.0(2) . . ? 
C13 C12 S11 117.3(2) . . ? 
C2 C12 S11 117.4(2) . . ? 
C12 C13 S17 124.2(2) . . ? 
C12 C13 S12 117.2(2) . . ? 
S17 C13 S12 118.33(13) . . ? 
C11 C14 S13 124.8(2) . . ? 
C11 C14 S14 121.7(2) . . ? 
S13 C14 S14 113.47(12) . . ? 
C16 C15 S15 125.4(2) . . ? 
C16 C15 S13 117.1(2) . . ? 
S15 C15 S13 117.42(13) . . ? 
C15 C16 S16 124.2(2) . . ? 
C15 C16 S14 116.8(2) . . ? 
S16 C16 S14 118.80(13) . . ? 
  
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 
 S7 C7 C3 C2 -81.1(3) . . . . ? 
 C7 C3 C2 C12 43.8(4) . . . . ? 
 C3 C2 C12 C13 89.9(3) . . . . ? 
 C2 C12 C13 S17 0.8(3) . . . . ? 
 C12 C13 S17 C17 -128.1(2) . . . . ? 
 C8A S5A C5 C6 116.4(3) . . . . ? 
 S5A C5 C6 S6 -19.5(4) . . . . ? 
 C5 C6 S6 C9 164.9(3) . . . . ? 
 C8B S5B C5 C6 -110.7(4) . . . . ? 
 C18 S15 C15 C16 -100.2(2) . . . . ? 
 S15 C15 C16 S16 -2.8(3) . . . . ? 
 C15 C16 S16 C19 145.8(2) . . . . ? 
  
_refine_diff_density_max    0.402 
_refine_diff_density_min   -0.511 
_refine_diff_density_rms    0.084 

#=============================================================END
 
data_8.ClO4 
  
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 4-bis(5-methyl-4',5'-ethylenedithiotetrathiafulvalenyl)
 perchlorate 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          
 'C18 H14 S12 1+, Cl O4 1-' 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum            'C18 H14 Cl O4 S12' 
_chemical_formula_weight          714.46 
_chemical_melting_point           ? 
_chemical_compound_source         ? 
  
_ccdc_compound_id                  '8.ClO4'
_ccdc_biological_activity          '?'
_ccdc_polymorph                    '?'
_ccdc_disorder                     
; the Cl, O1, O2, O3 atoms of the perchlorate anion are disordered
 between 2 positions, related via a twofold axis
;
_ccdc_comments               
 'cation radical salt, semiconductor'

loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'    .0181    .0091 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'    .0000    .0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'    .0492    .0322 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'S'  'S'    .3331    .5567 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Cl'  'Cl'    .3639    .7018 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
  
_symmetry_cell_setting            Orthorhombic 
_symmetry_space_group_name_H-M    P2(1)2(1)2 
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, -y, z' 
 '-x+1/2, y+1/2, -z' 
 'x+1/2, -y+1/2, -z' 
  
_cell_length_a                    11.074(3) 
_cell_length_b                    24.139(7) 
_cell_length_c                    4.876(2) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      1303.4(7) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     150(2) 
_cell_measurement_reflns_used     21 
_cell_measurement_theta_min       8.2 
_cell_measurement_theta_max       23.6 
  
_exptl_crystal_description        plate 
_exptl_crystal_colour             purple 
_exptl_crystal_size_max           0.30 
_exptl_crystal_size_mid           0.08 
_exptl_crystal_size_min           0.02 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.820 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              726 
_exptl_absorpt_coefficient_mu     10.545 
_exptl_absorpt_correction_type    psi-scan 
_exptl_absorpt_correction_T_min   0.5506 
_exptl_absorpt_correction_T_max   1.0000 
  
_exptl_special_details 
; 
 Absorption correction on 72 \y-scans of 2 reflections (TEXSAN 
 software); before it R(int)=0.114. 
; 
  
_diffrn_ambient_temperature       150(2) 
_diffrn_radiation_wavelength      1.54184 
_diffrn_radiation_type            CuK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device        'Rigaku AFC6S 4-circle diffractometer' 
_diffrn_measurement_method        '2\q/\w scans' 
_diffrn_standards_number          3 
_diffrn_standards_interval_count  150 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         0 
_diffrn_reflns_number             1429 
_diffrn_reflns_av_R_equivalents   0.0609 
_diffrn_reflns_av_sigmaI/netI     0.0822 
_diffrn_reflns_limit_h_min        -13 
_diffrn_reflns_limit_h_max        12 
_diffrn_reflns_limit_k_min        -30 
_diffrn_reflns_limit_k_max        27 
_diffrn_reflns_limit_l_min        -1 
_diffrn_reflns_limit_l_max        5 
_diffrn_reflns_theta_min          3.66 
_diffrn_reflns_theta_max          74.90 
_reflns_number_total              1288 
_reflns_number_observed           893 
_reflns_observed_criterion        >2sigma(I) 
  
_computing_data_collection        MSC/AFC 
_computing_cell_refinement        MSC/AFC 
_computing_data_reduction         TEXSAN 
_computing_structure_solution     'SHELXS-86 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)' 
_computing_molecular_graphics     SHELXTL 
_computing_publication_material   SHELXTL 
  
_refine_special_details 
; 
 Refinement on F^2^ for ALL reflections except for 11 with very negative 
F^2^ 
 or flagged by the user for potential systematic errors.  Weighted R-
factors 
 wR and all goodnesses of fit S are based on F^2^, conventional R-
factors R 
 are based on F, with F set to zero for negative F^2^. The observed 
criterion 
 of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. 
and is 
 not relevant to the choice of reflections for refinement. 
; 
  
_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme 
 'calc w=1/[\s^2^(Fo^2^)+(0.2335P)^2^+23.2910P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     constr 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_abs_structure_details 
 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    -0.04(24) 
_refine_ls_number_reflns          1277 
_refine_ls_number_parameters      129 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.1737 
_refine_ls_R_factor_obs           0.1276 
_refine_ls_wR_factor_all          0.4067 
_refine_ls_wR_factor_obs          0.3278 
_refine_ls_goodness_of_fit_all    1.063 
_refine_ls_goodness_of_fit_obs    1.098 
_refine_ls_restrained_S_all       1.122 
_refine_ls_restrained_S_obs       1.098 
_refine_ls_shift/esd_max          0.000 
_refine_ls_shift/esd_mean         0.000 
  
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_thermal_displace_type 
 _atom_site_occupancy 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_group 
S1 S 0.5505(6) 0.5785(2) 0.3884(21) 0.067(3) Uani 1 d . . 
S2 S 0.3277(5) 0.6124(3) 0.1202(16) 0.056(2) Uani 1 d . . 
S3 S 0.5596(6) 0.6962(3) 0.7111(16) 0.053(2) Uani 1 d . . 
S4 S 0.3271(5) 0.7266(3) 0.4628(15) 0.051(2) Uani 1 d . . 
S5 S 0.5709(6) 0.7941(3) 1.0745(16) 0.054(2) Uani 1 d . . 
S6 S 0.2900(6) 0.8266(4) 0.7898(17) 0.068(2) Uani 1 d . . 
C1 C 0.4418(26) 0.6303(11) 0.3523(63) 0.058(7) Uiso 1 d . . 
C2 C 0.4747(22) 0.5270(9) 0.1978(53) 0.043(6) Uiso 1 d . . 
C3 C 0.3712(25) 0.5441(13) 0.0586(79) 0.070(9) Uani 1 d . . 
C4 C 0.4427(21) 0.6786(9) 0.4798(53) 0.041(6) Uiso 1 d . . 
C5 C 0.4912(21) 0.7555(9) 0.8345(51) 0.039(6) Uiso 1 d . . 
C6 C 0.3801(22) 0.7702(10) 0.7261(60) 0.046(6) Uiso 1 d . . 
C7 C 0.2918(20) 0.5082(15) -0.1101(70) 0.076(10) Uani 1 d . . 
H71 H 0.2688(20) 0.5278(15) -0.2781(70) 0.114 Uiso 1 d R . 
H72 H 0.2190(20) 0.4988(15) -0.0053(70) 0.114 Uiso 1 d R . 
H73 H 0.3350(20) 0.4741(15) -0.1580(70) 0.114 Uiso 1 d R . 
C8 C 0.5118(26) 0.8620(10) 1.0007(58) 0.055(8) Uani 1 d . . 
H81 H 0.5531(26) 0.8896(10) 1.1182(58) 0.072 Uiso 1 d R . 
H82 H 0.5326(26) 0.8708(10) 0.8080(58) 0.072 Uiso 1 d R . 
C9 C 0.3758(20) 0.8690(11) 1.0264(75) 0.059(9) Uani 1 d . . 
H91 H 0.3547(20) 0.9085(11) 0.9986(75) 0.077 Uiso 1 d R . 
H92 H 0.3533(20) 0.8589(11) 1.2164(75) 0.077 Uiso 1 d R . 
Cl Cl 0.9833(14) 0.4923(6) 0.4086(24) 0.051(3) Uiso 0.50 d P . 
O1 O 1.0000 0.5000 0.1169(60) 0.058(7) Uiso 1 d S . 
O2 O 0.8918(34) 0.4551(15) 0.4638(95) 0.061(10) Uiso 0.50 d P . 
O3 O 0.9577(61) 0.5440(27) 0.5337(146) 0.115(24) Uiso 0.50 d P . 
O4 O 1.0943(48) 0.4662(20) 0.4940(119) 0.075(14) Uiso 0.50 d P . 
  
loop_ 
 _atom_site_aniso_label 
 _atom_site_aniso_U_11 
 _atom_site_aniso_U_22 
 _atom_site_aniso_U_33 
 _atom_site_aniso_U_23 
 _atom_site_aniso_U_13 
 _atom_site_aniso_U_12 
S1 0.046(4) 0.041(3) 0.113(7) 0.016(4) -0.033(5) -0.010(3) 
S2 0.028(3) 0.086(5) 0.053(4) 0.013(4) -0.006(3) 0.002(3) 
S3 0.036(3) 0.054(3) 0.070(5) 0.005(4) -0.013(4) -0.008(3) 
S4 0.034(3) 0.070(4) 0.049(4) 0.010(4) -0.009(3) 0.012(3) 
S5 0.040(3) 0.068(4) 0.055(4) 0.000(4) 0.002(3) -0.008(3) 
S6 0.045(4) 0.100(6) 0.058(5) -0.011(5) -0.005(4) 0.033(4) 
C3 0.039(15) 0.087(20) 0.085(25) -0.002(21) -0.001(18) -0.009(14) 
C7 0.012(12) 0.133(27) 0.083(22) -0.046(23) 0.003(15) 0.028(14) 
C8 0.067(18) 0.054(15) 0.044(15) 0.025(15) -0.021(16) 0.016(13) 
C9 0.022(12) 0.056(15) 0.099(26) 0.015(18) 0.024(16) -0.001(10) 
  
_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 1.74(3) . ? 
S1 C2 1.76(2) . ? 
S2 C3 1.74(3) . ? 
S2 C1 1.75(3) . ? 
S3 C5 1.73(2) . ? 
S3 C4 1.77(3) . ? 
S4 C4 1.73(2) . ? 
S4 C6 1.76(3) . ? 
S5 C5 1.74(2) . ? 
S5 C8 1.80(2) . ? 
S6 C6 1.72(3) . ? 
S6 C9 1.81(3) . ? 
C1 C4 1.32(3) . ? 
C2 C3 1.39(4) . ? 
C2 C2 1.42(5) 2_665 ? 
C3 C7 1.48(4) . ? 
C5 C6 1.39(3) . ? 
C8 C9 1.52(4) . ? 
Cl Cl 0.53(3) 2_765 ? 
Cl O3 1.25(6) 2_765 ? 
Cl O2 1.38(4) . ? 
Cl O4 1.39(5) 2_765 ? 
Cl O3 1.42(7) . ? 
Cl O4 1.44(5) . ? 
Cl O1 1.45(3) . ? 
Cl O2 1.90(4) 2_765 ? 
O1 Cl 1.45(3) 2_765 ? 
O2 O3 1.70(8) 2_765 ? 
O2 Cl 1.90(4) 2_765 ? 
O3 O4 0.65(8) 2_765 ? 
O3 Cl 1.25(6) 2_765 ? 
O3 O2 1.70(8) 2_765 ? 
O4 O3 0.65(8) 2_765 ? 
O4 Cl 1.39(5) 2_765 ? 
  
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 C2 97.1(12) . . ? 
C3 S2 C1 98.3(14) . . ? 
C5 S3 C4 95.7(11) . . ? 
C4 S4 C6 96.8(12) . . ? 
C5 S5 C8 99.7(13) . . ? 
C6 S6 C9 105.0(12) . . ? 
C4 C1 S1 125.5(23) . . ? 
C4 C1 S2 121.8(21) . . ? 
S1 C1 S2 112.8(15) . . ? 
C3 C2 C2 126.6(26) . 2_665 ? 
C3 C2 S1 116.1(20) . . ? 
C2 C2 S1 117.3(21) 2_665 . ? 
C2 C3 C7 125.8(28) . . ? 
C2 C3 S2 115.0(24) . . ? 
C7 C3 S2 119.0(23) . . ? 
C1 C4 S4 124.3(21) . . ? 
C1 C4 S3 121.1(20) . . ? 
S4 C4 S3 114.3(13) . . ? 
C6 C5 S3 117.9(20) . . ? 
C6 C5 S5 124.8(19) . . ? 
S3 C5 S5 117.2(14) . . ? 
C5 C6 S6 130.5(21) . . ? 
C5 C6 S4 115.0(19) . . ? 
S6 C6 S4 114.3(15) . . ? 
C9 C8 S5 116.4(20) . . ? 
C8 C9 S6 113.8(22) . . ? 
Cl Cl O3 97.5(45) 2_765 2_765 ? 
Cl Cl O2 168.1(23) 2_765 . ? 
O3 Cl O2 80.4(35) 2_765 . ? 
Cl Cl O4 85.5(40) 2_765 2_765 ? 
O3 Cl O4 133.2(34) 2_765 2_765 ? 
O2 Cl O4 87.5(27) . 2_765 ? 
Cl Cl O3 61.0(37) 2_765 . ? 
O3 Cl O3 120.7(58) 2_765 . ? 
O2 Cl O3 110.0(33) . . ? 
O4 Cl O3 27.0(31) 2_765 . ? 
Cl Cl O4 73.3(38) 2_765 . ? 
O3 Cl O4 27.0(35) 2_765 . ? 
O2 Cl O4 106.6(27) . . ? 
O4 Cl O4 139.3(42) 2_765 . ? 
O3 Cl O4 115.5(31) . . ? 
Cl Cl O1 79.5(6) 2_765 . ? 
O3 Cl O1 120.2(34) 2_765 . ? 
O2 Cl O1 111.7(21) . . ? 
O4 Cl O1 106.3(25) 2_765 . ? 
O3 Cl O1 109.5(30) . . ? 
O4 Cl O1 103.4(25) . . ? 
Cl Cl O2 8.6(17) 2_765 2_765 ? 
O3 Cl O2 91.1(34) 2_765 2_765 ? 
O2 Cl O2 160.6(34) . 2_765 ? 
O4 Cl O2 85.6(26) 2_765 2_765 ? 
O3 Cl O2 59.7(30) . 2_765 ? 
O4 Cl O2 68.3(23) . 2_765 ? 
O1 Cl O2 87.7(15) . 2_765 ? 
Cl O1 Cl 20.9(11) 2_765 . ? 
Cl O2 O3 46.5(26) . 2_765 ? 
Cl O2 Cl 3.3(6) . 2_765 ? 
O3 O2 Cl 46.1(26) 2_765 2_765 ? 
O4 O3 Cl 93.0(95) 2_765 2_765 ? 
O4 O3 Cl 73.7(83) 2_765 . ? 
Cl O3 Cl 21.5(17) 2_765 . ? 
O4 O3 O2 143.8(100) 2_765 2_765 ? 
Cl O3 O2 53.1(28) 2_765 2_765 ? 
Cl O3 O2 74.3(34) . 2_765 ? 
O3 O4 Cl 79.4(83) 2_765 2_765 ? 
O3 O4 Cl 60.0(79) 2_765 . ? 
Cl O4 Cl 21.3(13) 2_765 . ? 
  
_refine_diff_density_max    1.518 
_refine_diff_density_min    -.936 
_refine_diff_density_rms     .232 

#==============================================END