Evidence concerning the occurrence of a first-order phase transition around
260 K in the organic metal kappa-(BETS)(2)C(CN)(3) is reported and the eff
ect of the transition on the crystal and electronic structure of the salt i
s discussed. Determination of the crystal structure at 50 K has shown that
the main structural change brought about by the transition affects the anio
n sublattice. Although there are noticeable changes in the chalcogen . . .
chalcogen short contacts of the donor lattice it is shown that the Fermi su
rface is left unaltered by both the first-order transition and the thermal
contraction down to 50 K.