A study is presented on the synthesis and characterization of thernpentacyanoferrate(ll) complexes, NaJ[Fe(CN)sLr·.xH20 where L ~ p-nitroaniline,rno-nitroanline, p-nitrophenol, and o-nitrophenol. The structure of the synthesizedrncomplexes were confirmed by using IR, NMR, and UV-VIS spectroscopy andrncyclic-voltammetry measurements. Melting points were used to determine thernpurity of the synthesized complexes. Atomic absorption spectroscopy was used forrnthe analysis of sodium and iron and results confirmed the proposedrnstoichiometric formula of the complexes. Cyclic-voltammetric measurementsrnindicated the occurrence of one reversible wave for each complex. These werernassigned to the oxidation of Fe(ll) and reduction of Fe(1I1) in the reversible waverncycle. Low solid conductivity of the complexes were observed. This is related tornthe strength of the iron (II) - cyanide bond.