The reaction of tricyanometallate precursor, (Bu 4 N)[(Tp*)Fe(CN) 3 ] (Tp*=hydrotris(3,5-dimethylpyrazol-l-yl)borate) with Co(ClO 4 ) 2 ·6H 2 O in the presence of the bidentate dpa (dpa=2,2′-dipyridyl amine) ligand affords one novel cyano-bridged heterobimetallic {Fe 2 Co 2 } molecular square, [Fe III (Tp*)(CN) 3 ] 2 [Co II (dpa) 2 ] 2 •2ClO 4 •4H 2 O•4CH 3 OH (1). The molecular structure was determined by single-crystal X-ray diffraction. In compound 1, Fe III ion is coordinated by three cyanide carbon atoms and three nitrogen atoms of Tp* anions. Whereas, the Co II ion is surrounded by two cyanide nitrogen atoms and four nitrogen atoms from two bidentate dpa ligands. Cyclic voltammetry (CV) measurements showed that complex 1 exhibited one quasi-reversible waves (0.1V vs SCE) in the reduction process, and irreversible waves in the oxidation process. Magnetic measurements indicate that complex 1 exhibits a strong intramolecular ferromagnetic interaction between the low-spin Fe III (S=1/2) and high-spin Co II (S=3/2) ions.