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Abstract

4.5-Dimethyl-4'.5'-ethylenedithiolotetrathiafulvalene (DIMET) was obtained by reacting 4.5- ethylenedithiolo-1.3-dithioliumtetrafluoroborate with 4.5-dimethyl- 1.3-dithiolium-tetrafluoroborate in the presence of diisopropylethylamine or triethylamine. Electrocrystallization of this donor in different solvents like dichloromethane or tetrahydrofurane (THF) and with varying supporting electrolytes, like tetrabutylammonium hexafluorophosphate, triiodide, nitrate, perrhenate or perchlorate, results in a large number of well crystallizing compounds. The crystal and molecular structure of one of the isolated solids was elucidated by X-ray methods.

(C10)H10S6)2CIO4 x C4H8O, Mr = 816.66, is triclinic, P1̄ , a = 6.731(5), b - 7.632(3), c = 33.32(3) Å , α = 96.53(5), β = 92.99(6), γ = 103.13(5)°, V - 1650.7 Å3, Z = 2, dc = 1.64 gem-3, final Rw = 0.077 for 1844 observed independent reflections. Sheets of cations with an average charge of 1/2+ are separated by sheets of anions and THF solvent molecules. Intermolecular S···S contacts result in two-dimensional physical properties. Electrical conductivity and thermopower measurements indicate two broad phase transitions at around 200 K and 80 K