Pt nanoclusters have been generated by reaction of Pt vapour and mesitylene vapour and the role of the mesitylene/platinum ratio and the Pt particle size has been evaluated, quenching the resulting mesitylene solvated Pt atoms with 1,3-divinyltetramethyldisiloxane (DVS) as additional ligand. The Pt particle sizes have been estimated on the basis of DOSY (Diffusion-Ordered SpectroscopY) analysis and information on their structure features have been obtained by combined use of 2D NMR techniques.