We report herein the spectroscopic (FTIR, NMR and UV-Vis) and electrochemical (Cyclic Voltammetry) studies of new compounds of general formula [MCp(L2)(CC{SC4H2}2NO2)] (M=Fe, Ru; L2=dppe or 2 PPh3). Electrochemical and spectroscopic data will be analyzed in order to give an insight on the second-order nonlinear optical properties of these compounds.