A new charge-transfer coordination compound [(C5S5H3CH2O)4Ni](FeCp2)0.84 was synthesized in this work. The molecular formula of the coordination compound was confirmed by elementary analysis and ICP. The structure of this compound was defined by 1HNMR, IR and UV-Vis. Electrochemical properties of the new compound were studied by cyclic voltammetry (CV). Electrical property was tested by four probe methods with R-T curve.