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The structure of the electrochemically crystallized title compound, (C10H8S8)3[CoCl4]2, consists of two types of bis­(ethyl­enedithio)tetra­thia­fulvalene (BEDT-TTF) radical cation stacks separated by sheets of tetra­hedral [CoCl4]2− anions. One of the BEDT-TTF mol­ecules is generated by inversion. There are short S...S contacts between the stacks in the a direction and short C—H...Cl contacts between the radical cations and the anions.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536808033692/hb2784sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536808033692/hb2784Isup2.hkl
Contains datablock I

CCDC reference: 712283

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.022 Å
  • R factor = 0.100
  • wR factor = 0.281
  • Data-to-parameter ratio = 17.9

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT026_ALERT_3_B Ratio Observed / Unique Reflections too Low .... 37 Perc. PLAT250_ALERT_2_B Large U3/U1 Ratio for Average U(i,j) Tensor .... 4.15 PLAT341_ALERT_3_B Low Bond Precision on C-C Bonds (x 1000) Ang ... 22
Alert level C Value of measurement temperature given = 293.000 Value of melting point given = 0.000 RFACG01_ALERT_3_C The value of the R factor is > 0.10 R factor given 0.100 RFACR01_ALERT_3_C The value of the weighted R factor is > 0.25 Weighted R factor given 0.281 PLAT084_ALERT_2_C High R2 Value .................................. 0.28 PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.96 Ratio PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C10 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C12 PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 3.00 PLAT360_ALERT_2_C Short C(sp3)-C(sp3) Bond C9 - C10 ... 1.42 Ang. PLAT431_ALERT_2_C Short Inter HL..A Contact Cl1 .. S2 .. 3.39 Ang. PLAT431_ALERT_2_C Short Inter HL..A Contact Cl2 .. S12 .. 3.37 Ang. PLAT431_ALERT_2_C Short Inter HL..A Contact Cl3 .. S12 .. 3.27 Ang. PLAT431_ALERT_2_C Short Inter HL..A Contact Cl3 .. S11 .. 3.30 Ang. PLAT431_ALERT_2_C Short Inter HL..A Contact Cl3 .. S9 .. 3.43 Ang. PLAT431_ALERT_2_C Short Inter HL..A Contact Cl4 .. S7 .. 3.29 Ang. PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT066_ALERT_1_C Predicted and Reported Transmissions Identical . ? PLAT720_ALERT_4_C Number of Unusual/Non-Standard Labels .......... 1 PLAT731_ALERT_1_C Bond Calc 1.52(3), Rep 1.527(10) ...... 3.00 su-Ra C11 -C12 1.555 1.555
Alert level G FORMU01_ALERT_1_G There is a discrepancy between the atom counts in the _chemical_formula_sum and _chemical_formula_moiety. This is usually due to the moiety formula being in the wrong format. Atom count from _chemical_formula_sum: C30 H24 Cl8 Co2 S24 Atom count from _chemical_formula_moiety:C30 H24 Cl8 Co2 S243 PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 8 PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
0 ALERT level A = In general: serious problem 3 ALERT level B = Potentially serious problem 18 ALERT level C = Check and explain 4 ALERT level G = General alerts; check 6 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 13 ALERT type 2 Indicator that the structure model may be wrong or deficient 5 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Comment top

There is a large variety of quasi-two-dimensional organic conductors based on the radical cation salts of bis(ethylenedithio)tetrathiafulvalene (BEDT-TTF) which also is abbreviated to ET. They show a wealth of structural modifications, but the conducting properties of the radical salts are essentially determined by the packing patterns of their BEDT-TTF layers (Shibaeva & Yagubskii, 2004). So, according to packing patterns of the BEDT-TTF layers in the various crystal structure, it is customary classified as α, β, δ, χ and so on. (Mori, 1998; Mori, 1999; Mori et al., 1999)

In the title structure, (I), the unit cell contains three ET donors and two anions. Since one BEDT-TTF molecule (ETA) and [CoCl4]2- anion are on general positions, and the other BEDT-TTF molecule (ETB) is positioned on an inversion center, the crystallographically independent molecules are 1.5 ET molecules and one [CoCl4]2- anion (Fig. 1). The [CoCl4]2- anion shows a slightly distorted tetrahedral configuration (Table 1). The two independent ET molecules have different molecular configuration. In the ETA, the terminal ethylene C2 and C9 atoms extend from the molecular plane with deviations of -0.499 (16) Å and -0.579 (18) Å, but C1 and C10 atoms [with deviations of 0.169 (17) Å and 0.057 (19) Å] almost share the same plane with the rest of the molecule. ETA shows a boat conformation in which C2 and C9 are on the both sides of the molecular plane. Otherwise, ETB shows a chair conformation in which C11 and C12 deviate from the molecular plane by 0.658 (18) Å and 0.02 (2) Å respectively and the inversion center positioned on the middle of the C15—C15A bond. The dihedral angle between the molecular planes of ETA and ETB is 16.88 (16)° and their molecular planes make angles of 43.93 (10)° and 27.10 (13)° with [010] directions respectively.

ETA and ETB form stack A and stack B along the b axis in a face to face manner with different intra-stack packing modes. In the stack A, ETA molecules are dimerized and the intra-stack packing mode alternates between the ROB [ring over bond, ET molecules stack on top of each other with a relative displacement between stacking moleculaes along their long in-plane axes] and ROA [ring over atom, ET molecules stack on above or below with a large displacement betweentacking moleculaes along their short in-plane axes] modes, as defined by Williams et al. (1984). The mean interplannar distance in the dimersied ET molecules is 3.606 Å and between the dimerized is 3.082 Å. There are three kinds of intra-dimer S···S short distances within each dimmer shorter than the combined van der Walls radii of two sulfur atoms (3.60 Å), but there are no obvious inter-dimer S···S short contacts between the dimers. Stack B contains only ETB molecules overlapped with ROB mode, and there are no intrastack S···S short contacts. The mean interplannar distance in stack B is 4.392 Å.

Stack A and Stack B form layer A and layer B in the ab plane respectively and these layers are interleaved by the inorganic anions. In layer A, one ET molecule has four pairs of inter-stack S···S short contacts between the stacks in the a-direction [S1···S2 = 3.518 (6) Å, S1···S4 = 3.562 (6) Å, S7···S8 = 3.549 (6) Å] as shown in Fig. 2. Combined with intra-stack S···S short contacts within Stack A, it is suggested that the possibility of a quasi-two-dimensional interaction in the ab-plane. In contrast to the layer A, there are no S···S distance are shorter than the sum of van der Walls radii of two sulfur atoms in the layer B, which indicates the absence of any intermolecular interaction in the layer B.

Between layer A and layer B, there are layers of [CoCl4]2- anions, which engage in ionic donor-anion interactions. The anions sandwich the layers A and layers B along the c axis. The [CoCl4]2- anions are situated in the so called 'anion cavity', which is bonded by the terminal ethylene groups of the ET cations. Short C—H···Cl interactions (Table 2) probably stabilize the crystal structure.

Among the molecular conductors based on the ET, there are three major determinant of packing of a crystal: (1) the ET network packing motif; (2) the anion layer motif; and (3) the interatomic environment at the interface of the donor and anion layers. For the larger size of the ET and fractional charge on it, the coulomb interaction between the ET cations and anions is inferior to the π-π interaction. In the title crystal, the ET molecules form poly-ET cations by the π-π interaction and [CoCl4]2- anions fill the cavity formed by the ethylene groups of the surrounding ET molecules to balance charge. Hence, the 'anion cavity' is mainly determined by the ET packing motif where the 'anion cavity' is a trigonal channel along the [100] directions. If the size of anion is not enough to fill the anion cavity, the solvent molecules will be crystallized in the crystal to stabilize the structure, such as TCE(1,1,2-trichloroethane) molecules in the crystal α-ET3(CoCl4)(TCE)(Mori et al., 2002). In the crystal α-ET3(CoCl4)(TCE), the oxidation on ET molecules is lower than that in the title compound, where only one [CoCl4]2- anion is needed to balance charge, so the TCE solvent molecules are filled in the 'anion cavity' together. At the same time, if some of the anions are replaced by the other anion with same geometry, size and charge, the crystal structure will be an isomorphic structure, for example, β-(ET)3(CoCl4)1.34(GaCl4)0.66, α-ET3(CoCl4)0.38(CoCl4)0.62(TCE) (Mori et al., 2002). On the other hand, the oxidation on ET molecules and the interaction between the anions and the ethylene groups of the ET will significant affect the packing motif of the ET cations, so the ET packing motif of the title crystal belongs to β' and ET3(CoCl4)(TCE) belongs to α. But the 'anion cavity' formed by the ET cations as above two packing motif are nearly same.

Related literature top

For related literature, see: Mori (1998, 1999); Mori et al. (1999, 2002); Shibaeva & Yagubskii (2004); Varma et al. (1987); Williams et al. (1984).

Experimental top

BEDT-TTF was synthesized following the method of Varma et al. (1987) and recrystallized from CHCl3. K2CoCl4.6H2O was synthesized by metathesis of CoCl2.6H2O and KCl in a molar ratio of 1:2 in water and recrystallized before use. All solvent were distilled before use.

Electrochemical crystal growth was carried out in conventional H-shaped cells with Pt electrodes in a constant temperature of 295 (2) K at a current of 0.2 µA. Each cell contained 7 mg of BEDT-TTF and 99.3 mg of K2CoCl4.6H2O together with 40 mg of 18-crown-6 in 35 mL of TCE(1,1,2-trichloroethane) under an inert atmosphere (N2). Black needles of (I) were obtained after three months.

Refinement top

The electrocrystallization process is a 'self-assembly' process which is difficult to control. The tendency to grow as bundles of fine needles has hampered our efforts to get a better crystal. The low quality of the crystal was the reason for low bond precision, but the obtained structure information of the title compound is meaningful.

The H atoms were geometrically placed (C—H = 0.97Å) and refined as riding with Uiso(H)= 1.2 Ueq(C).

Computing details top

Data collection: XSCANS (Bruker, 1996); cell refinement: XSCANS (Bruker, 1996); data reduction: XSCANS (Bruker, 1996); program(s) used to solve structure: SIR (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. Molecular structure of (I) with displacement ellipsoids for the non-hydrogen atoms at the 30% probability level. The unlabelled atoms of the ETB molecule are generated by the symmetry operation (1-x, 1-y, 1-x).
[Figure 2] Fig. 2. A packing diagram of (I), with short S···S contacts indicated by dashed lines. The anions and H atoms are omitted for clarity.
Bis(ethylenedithio)tetrathiafulvalenium–tetrachloridocobaltate(II) (3/2) top
Crystal data top
(C10H8S8)3[CoCl4]2Z = 1
Mr = 1555.39F(000) = 778
Triclinic, P1Dx = 1.969 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 6.7904 (19) ÅCell parameters from 31 reflections
b = 9.6402 (18) Åθ = 5.0–12.4°
c = 20.499 (4) ŵ = 2.03 mm1
α = 86.280 (14)°T = 293 K
β = 89.967 (19)°Prism, black
γ = 78.456 (19)°0.22 × 0.18 × 0.10 mm
V = 1311.9 (5) Å3
Data collection top
Bruker P4
diffractometer
1927 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.094
Graphite monochromatorθmax = 26.0°, θmin = 2.0°
/w scansh = 81
Absorption correction: ψ scan
(XSCANS; Bruker, 1996)
k = 1111
Tmin = 0.652, Tmax = 0.816l = 2525
6527 measured reflections97 standard reflections every 3 reflections
5159 independent reflections intensity decay: 1%
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.100Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.281H-atom parameters constrained
S = 0.92 w = 1/[σ2(Fo2) + (0.1192P)2]
where P = (Fo2 + 2Fc2)/3
5159 reflections(Δ/σ)max < 0.001
289 parametersΔρmax = 0.91 e Å3
8 restraintsΔρmin = 1.06 e Å3
Crystal data top
(C10H8S8)3[CoCl4]2γ = 78.456 (19)°
Mr = 1555.39V = 1311.9 (5) Å3
Triclinic, P1Z = 1
a = 6.7904 (19) ÅMo Kα radiation
b = 9.6402 (18) ŵ = 2.03 mm1
c = 20.499 (4) ÅT = 293 K
α = 86.280 (14)°0.22 × 0.18 × 0.10 mm
β = 89.967 (19)°
Data collection top
Bruker P4
diffractometer
1927 reflections with I > 2σ(I)
Absorption correction: ψ scan
(XSCANS; Bruker, 1996)
Rint = 0.094
Tmin = 0.652, Tmax = 0.81697 standard reflections every 3 reflections
6527 measured reflections intensity decay: 1%
5159 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.1008 restraints
wR(F2) = 0.281H-atom parameters constrained
S = 0.92Δρmax = 0.91 e Å3
5159 reflectionsΔρmin = 1.06 e Å3
289 parameters
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
C110.271 (3)0.0230 (19)0.6376 (9)0.068 (6)
H11A0.26240.09860.66710.081*
H11B0.18450.03970.65420.081*
C120.487 (2)0.0600 (19)0.6370 (11)0.085 (7)
H12A0.49170.13790.60900.102*
H12B0.52260.10130.68090.102*
C10.557 (2)0.4107 (18)1.1811 (8)0.051 (5)
H1A0.67580.34131.19520.061*
H1B0.51160.46651.21800.061*
C20.397 (2)0.3341 (16)1.1632 (8)0.041 (4)
H2A0.38160.26801.19970.049*
H2B0.44430.27841.12650.049*
C30.397 (2)0.5999 (16)1.0767 (7)0.035 (4)
C40.218 (2)0.5659 (13)1.0853 (7)0.029 (3)
C50.161 (2)0.7692 (15)0.9978 (7)0.035 (4)
C60.076 (2)0.8723 (13)0.9480 (7)0.023 (3)
C70.023 (2)1.0697 (16)0.8548 (7)0.035 (4)
C80.155 (2)1.0292 (14)0.8635 (7)0.034 (4)
C90.106 (3)1.2069 (19)0.7415 (9)0.061 (6)
H9A0.09771.28490.70990.073*
H9B0.08271.12090.71810.073*
C100.304 (3)1.228 (2)0.7659 (9)0.069 (6)
H10A0.39531.24540.72860.082*
H10B0.32601.31510.78880.082*
C130.350 (2)0.2161 (15)0.5480 (7)0.035 (4)
C140.542 (2)0.1863 (16)0.5711 (8)0.040 (4)
C150.485 (3)0.4319 (15)0.5147 (9)0.045 (4)
Cl10.0026 (7)0.7913 (4)0.7470 (2)0.0460 (11)
Cl20.2946 (7)0.5703 (5)0.6666 (2)0.0563 (13)
Cl30.0831 (8)0.7338 (5)0.5751 (2)0.0546 (13)
Cl40.2378 (7)0.4170 (4)0.6910 (2)0.0529 (12)
Co010.0140 (4)0.6252 (2)0.67099 (11)0.0402 (6)
S10.6258 (6)0.5265 (5)1.1162 (2)0.0508 (13)
S20.1496 (6)0.4391 (4)1.1417 (2)0.0426 (11)
S30.4092 (6)0.7397 (4)1.0199 (2)0.0373 (10)
S40.0217 (6)0.6592 (4)1.0356 (2)0.0351 (10)
S50.2191 (6)0.9787 (4)0.9081 (2)0.0371 (10)
S60.1704 (6)0.9004 (4)0.9241 (2)0.0370 (10)
S70.0938 (6)1.1928 (4)0.7998 (2)0.0388 (11)
S80.3763 (6)1.0934 (5)0.8193 (2)0.0439 (11)
S90.1832 (8)0.0971 (5)0.5591 (2)0.0572 (14)
S100.6771 (8)0.0341 (5)0.6107 (3)0.0673 (16)
S110.2669 (7)0.3772 (5)0.5071 (2)0.0536 (13)
S120.6655 (6)0.3251 (4)0.5600 (2)0.0450 (12)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C110.089 (17)0.062 (13)0.058 (13)0.042 (13)0.003 (12)0.028 (10)
C120.104 (18)0.063 (13)0.098 (17)0.053 (14)0.022 (14)0.035 (12)
C10.038 (10)0.046 (10)0.060 (12)0.004 (9)0.018 (9)0.028 (9)
C20.028 (9)0.030 (9)0.060 (11)0.002 (7)0.011 (8)0.018 (8)
C30.047 (10)0.037 (9)0.025 (8)0.024 (8)0.011 (8)0.012 (7)
C40.039 (9)0.014 (7)0.031 (8)0.006 (7)0.001 (7)0.011 (6)
C50.039 (10)0.029 (8)0.042 (9)0.023 (8)0.015 (8)0.014 (7)
C60.024 (8)0.017 (7)0.028 (8)0.005 (6)0.003 (7)0.007 (6)
C70.027 (9)0.032 (8)0.040 (10)0.007 (7)0.007 (8)0.008 (7)
C80.040 (10)0.018 (7)0.044 (10)0.008 (7)0.001 (8)0.010 (7)
C90.065 (13)0.054 (12)0.074 (13)0.048 (11)0.022 (11)0.025 (10)
C100.040 (12)0.090 (16)0.074 (14)0.023 (12)0.020 (11)0.035 (12)
C130.041 (10)0.029 (8)0.036 (9)0.010 (8)0.013 (8)0.013 (7)
C140.031 (9)0.030 (8)0.060 (11)0.016 (7)0.013 (8)0.026 (8)
C150.043 (10)0.021 (8)0.069 (12)0.009 (8)0.000 (9)0.011 (8)
Cl10.058 (3)0.028 (2)0.053 (3)0.013 (2)0.001 (2)0.0053 (18)
Cl20.053 (3)0.047 (3)0.071 (3)0.020 (2)0.004 (3)0.013 (2)
Cl30.071 (3)0.045 (3)0.050 (3)0.021 (2)0.003 (2)0.013 (2)
Cl40.047 (3)0.031 (2)0.077 (3)0.006 (2)0.002 (2)0.016 (2)
Co010.0444 (15)0.0261 (11)0.0492 (14)0.0093 (11)0.0038 (12)0.0124 (10)
S10.030 (2)0.044 (3)0.076 (3)0.011 (2)0.013 (2)0.028 (2)
S20.035 (2)0.032 (2)0.060 (3)0.014 (2)0.002 (2)0.024 (2)
S30.032 (2)0.038 (2)0.044 (2)0.0170 (19)0.005 (2)0.0166 (18)
S40.030 (2)0.027 (2)0.048 (3)0.0129 (18)0.0060 (19)0.0179 (17)
S50.030 (2)0.031 (2)0.050 (3)0.0120 (18)0.004 (2)0.0195 (18)
S60.030 (2)0.030 (2)0.053 (3)0.0170 (18)0.007 (2)0.0143 (18)
S70.033 (2)0.035 (2)0.047 (3)0.011 (2)0.002 (2)0.0167 (19)
S80.034 (2)0.043 (2)0.053 (3)0.012 (2)0.010 (2)0.019 (2)
S90.060 (3)0.052 (3)0.065 (3)0.034 (3)0.014 (3)0.030 (2)
S100.058 (3)0.030 (2)0.105 (4)0.003 (2)0.008 (3)0.030 (3)
S110.041 (3)0.044 (3)0.075 (3)0.019 (2)0.015 (2)0.031 (2)
S120.035 (2)0.038 (2)0.062 (3)0.015 (2)0.009 (2)0.018 (2)
Geometric parameters (Å, º) top
C11—C121.527 (10)C7—C81.35 (2)
C11—S91.772 (17)C7—S71.723 (14)
C11—H11A0.9700C7—S51.774 (15)
C11—H11B0.9700C8—S61.717 (14)
C12—S101.782 (9)C8—S81.735 (16)
C12—H12A0.9700C9—C101.42 (2)
C12—H12B0.9700C9—S71.786 (17)
C1—C21.49 (2)C9—H9A0.9700
C1—S11.803 (16)C9—H9B0.9700
C1—H1A0.9700C10—S81.791 (17)
C1—H1B0.9700C10—H10A0.9700
C2—S21.818 (15)C10—H10B0.9700
C2—H2A0.9700C13—C141.36 (2)
C2—H2B0.9700C13—S111.708 (14)
C3—C41.333 (19)C13—S91.771 (15)
C3—S31.738 (14)C14—S121.719 (14)
C3—S11.747 (16)C14—S101.720 (15)
C4—S41.739 (14)C15—C15i1.46 (3)
C4—S21.756 (13)C15—S121.672 (17)
C5—C61.416 (18)C15—S111.679 (16)
C5—S31.708 (15)Co1—Cl12.296 (5)
C5—S41.708 (13)Co1—Cl22.265 (5)
C6—S61.706 (14)Co1—Cl32.259 (5)
C6—S51.720 (13)Co1—Cl42.276 (5)
C12—C11—S9112.6 (14)S6—C8—S8115.0 (9)
C12—C11—H11A109.1C10—C9—S7117.0 (15)
S9—C11—H11A109.1C10—C9—H9A108.0
C12—C11—H11B109.1S7—C9—H9A108.0
S9—C11—H11B109.1C10—C9—H9B108.0
H11A—C11—H11B107.8S7—C9—H9B108.0
C11—C12—S10117.6 (12)H9A—C9—H9B107.3
C11—C12—H12A107.9C9—C10—S8119.3 (14)
S10—C12—H12A107.9C9—C10—H10A107.5
C11—C12—H12B107.9S8—C10—H10A107.5
S10—C12—H12B107.9C9—C10—H10B107.5
H12A—C12—H12B107.2S8—C10—H10B107.5
C2—C1—S1114.6 (12)H10A—C10—H10B107.0
C2—C1—H1A108.6C14—C13—S11117.8 (11)
S1—C1—H1A108.6C14—C13—S9123.2 (11)
C2—C1—H1B108.6S11—C13—S9119.0 (9)
S1—C1—H1B108.6C13—C14—S12113.9 (11)
H1A—C1—H1B107.6C13—C14—S10130.2 (11)
C1—C2—S2117.9 (11)S12—C14—S10115.8 (9)
C1—C2—H2A107.8C15i—C15—S12121.2 (17)
S2—C2—H2A107.8C15i—C15—S11122.1 (17)
C1—C2—H2B107.8S12—C15—S11116.7 (8)
S2—C2—H2B107.8Cl3—Co01—Cl2110.4 (2)
H2A—C2—H2B107.2Cl3—Co01—Cl4110.28 (19)
C4—C3—S3116.7 (12)Cl2—Co01—Cl4106.69 (18)
C4—C3—S1129.2 (11)Cl3—Co01—Cl1105.49 (17)
S3—C3—S1114.1 (8)Cl2—Co01—Cl1107.4 (2)
C3—C4—S4116.9 (10)Cl4—Co01—Cl1116.55 (19)
C3—C4—S2128.5 (12)C3—S1—C1103.6 (7)
S4—C4—S2114.6 (8)C4—S2—C299.8 (7)
C6—C5—S3122.8 (10)C5—S3—C395.1 (7)
C6—C5—S4120.8 (11)C5—S4—C495.0 (7)
S3—C5—S4116.3 (8)C6—S5—C795.2 (7)
C5—C6—S6123.3 (10)C6—S6—C896.0 (7)
C5—C6—S5120.7 (11)C7—S7—C998.3 (8)
S6—C6—S5116.0 (8)C8—S8—C10101.3 (8)
C8—C7—S7131.0 (12)C13—S9—C1197.4 (8)
C8—C7—S5114.8 (11)C14—S10—C12103.2 (8)
S7—C7—S5114.2 (9)C15—S11—C1394.8 (7)
C7—C8—S6118.0 (12)C15—S12—C1496.2 (7)
C7—C8—S8127.0 (11)
S9—C11—C12—S1061 (2)C3—C4—S4—C53.4 (14)
S1—C1—C2—S263.6 (17)S2—C4—S4—C5175.8 (9)
S3—C3—C4—S43.4 (18)C5—C6—S5—C7178.4 (12)
S1—C3—C4—S4178.5 (10)S6—C6—S5—C72.0 (9)
S3—C3—C4—S2175.7 (9)C8—C7—S5—C60.7 (14)
S1—C3—C4—S22 (2)S7—C7—S5—C6178.4 (9)
S3—C5—C6—S6178.5 (9)C5—C6—S6—C8178.0 (13)
S4—C5—C6—S62.7 (19)S5—C6—S6—C82.4 (9)
S3—C5—C6—S51.9 (18)C7—C8—S6—C62.0 (14)
S4—C5—C6—S5177.7 (8)S8—C8—S6—C6177.8 (9)
S7—C7—C8—S6179.7 (10)C8—C7—S7—C918.6 (19)
S5—C7—C8—S60.9 (18)S5—C7—S7—C9160.3 (10)
S7—C7—C8—S80 (3)C10—C9—S7—C749.3 (16)
S5—C7—C8—S8178.9 (9)C7—C8—S8—C103.3 (18)
S7—C9—C10—S864 (2)S6—C8—S8—C10176.9 (10)
S11—C13—C14—S124.6 (19)C9—C10—S8—C835.6 (19)
S9—C13—C14—S12174.7 (9)C14—C13—S9—C1134.6 (17)
S11—C13—C14—S10176.7 (11)S11—C13—S9—C11144.8 (10)
S9—C13—C14—S104 (3)C12—C11—S9—C1364.9 (14)
C4—C3—S1—C18.6 (18)C13—C14—S10—C1217 (2)
S3—C3—S1—C1169.6 (9)S12—C14—S10—C12161.7 (11)
C2—C1—S1—C337.9 (15)C11—C12—S10—C1417 (2)
C3—C4—S2—C217.8 (17)C15i—C15—S11—C13177 (2)
S4—C4—S2—C2163.1 (9)S12—C15—S11—C135.1 (12)
C1—C2—S2—C449.0 (14)C14—C13—S11—C150.1 (15)
C6—C5—S3—C3176.9 (13)S9—C13—S11—C15179.5 (11)
S4—C5—S3—C30.9 (11)C15i—C15—S12—C14175 (2)
C4—C3—S3—C51.4 (14)S11—C15—S12—C147.2 (12)
S1—C3—S3—C5179.9 (9)C13—C14—S12—C156.9 (15)
C6—C5—S4—C4178.4 (13)S10—C14—S12—C15174.3 (11)
S3—C5—S4—C42.3 (11)
Symmetry code: (i) x+1, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C1—H1A···Cl1ii0.972.553.494 (16)165
C1—H1B···Cl2iii0.972.833.591 (16)136
C10—H10A···Cl4iv0.972.783.57 (2)139
Symmetry codes: (ii) x+1, y+1, z+2; (iii) x, y+1, z+2; (iv) x1, y+1, z.

Experimental details

Crystal data
Chemical formula(C10H8S8)3[CoCl4]2
Mr1555.39
Crystal system, space groupTriclinic, P1
Temperature (K)293
a, b, c (Å)6.7904 (19), 9.6402 (18), 20.499 (4)
α, β, γ (°)86.280 (14), 89.967 (19), 78.456 (19)
V3)1311.9 (5)
Z1
Radiation typeMo Kα
µ (mm1)2.03
Crystal size (mm)0.22 × 0.18 × 0.10
Data collection
DiffractometerBruker P4
diffractometer
Absorption correctionψ scan
(XSCANS; Bruker, 1996)
Tmin, Tmax0.652, 0.816
No. of measured, independent and
observed [I > 2σ(I)] reflections
6527, 5159, 1927
Rint0.094
(sin θ/λ)max1)0.617
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.100, 0.281, 0.92
No. of reflections5159
No. of parameters289
No. of restraints8
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.91, 1.06

Computer programs: XSCANS (Bruker, 1996), SIR (Altomare et al., 1999), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Selected bond lengths (Å) top
Co1—Cl12.296 (5)Co1—Cl32.259 (5)
Co1—Cl22.265 (5)Co1—Cl42.276 (5)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C1—H1A···Cl1i0.972.553.494 (16)165
C1—H1B···Cl2ii0.972.833.591 (16)136
C10—H10A···Cl4iii0.972.783.57 (2)139
Symmetry codes: (i) x+1, y+1, z+2; (ii) x, y+1, z+2; (iii) x1, y+1, z.
 

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