Nanoparticles of the Per2[Au(mnt)2] (Per perylene; mnt2- maleonitrile dithiolate) compound have been obtained by the electrochemical oxidation of perylene in the presence of [(n-C4H9)4N][Au(mnt)2] and, either an amphiphilic molecule (OATM), or a zwitterionic ionic liquid (BIBS), acting as growth controlling agents. When the reaction is carried out with OATM, nanocrystals exhibiting sizes in the 35–100 nm range are grown whereas roughly spherical nanoparticles are observed if BIBS is used (10–40 nm in diameter). Infrared and Raman spectra confirm the presence of both perylene donor and maleonitrile dithiolate ligands within the nanopowders. Electrical conductivity measurements at room temperature lead to about 0.025 S.cm-1, a typical value for nanopowders of bis(dithiolene)-based conducting compounds. Finally, current–voltage characteristics for the spherical nanoparticles are fitted with a Shockley diode model. A saturation current of 19.3 pA and a threshold voltage of 0.149 V are extracted from this model.