A single crystal of [P(C6H5)(4)][(MnFeIII)-Fe-II(C2O4)(3)] was synthesized
and structurally characterized by X-ray; space group is R3c, a = 18.881(2),
c = 57.320(10) Angstrom. X-ray diffraction and Mossbauer studies suggested
dynamical disorder for the organic cation located on the threefold axis. T
he order-disorder phase transition at ca. 330 K is associated with the orie
ntational disorder of the P(C6H5)(4)(+) cation occupying a general position
in the crystal.