We have studied the morphology, the Structure and the chemical composition of micro- and nano-structures grown by electron beam-induced deposition of [RhCl(PF3)(2)](2). Transmission electron microscopy revealed that the deposits are made up of face centered cubic crystalline Rh grains (4-6 nm in diameter) immersed in an amorphous matrix. Auger electron spectroscopy and electron energy loss spectroscopy showed that a carbon contamination layer is present at the deposit surface, while the bulk material contains the elements Rh (60at%), P (20at%), Cl, O and N (remaining 20 at%). The structure. the chemical composition of the deposits and the size of the Rh nano-crystals are independent of the deposit shape and of the deposition parameters, within the range explored in this work. (C) 2004 Elsevier B.V. All rights reserved.