Electrical oxidation of bis(ethylenedithiolo)tetrathiofulvalene (BEDT-TTF) 1 in a nitrogen saturated tetrahydrofurane solution containing (n-C4HIO)4N+I:i' as electrolyte results in the deposition of crystal plates of (BEpT-TTF)rI3' (CIOHgSshI3' These two dimensional crystals are triclinic, space group PI, a = 9.211(2), b = 1O.S50 ( 4) behave like a two dimensional metal. while below 135 K a metal-insolator transition occurs. The thermopower values indicate that the high temperature conductivity is dominated by holes. An estimate of the Fermi energy (F gives a value of (F '" 0.3 eV.
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