A new compound, [Cu 4 (bix) 3 V 4 O 12 ] (1) (bix=1,4-Bis(imidazol-1-ylmethyl)benzene), has been hydrothermally synthesized, and characterized by elemental analyses, IR spectroscopy, thermogravimetric analysis, and single X-ray diffraction. In the structure of compound 1, the 2D layer is constructed from the ladder-like chains in which the [V 4 O 12 ] 4− polyanions act as the middle rails. The whole structure exhibits an interdigitated architecture which is unusual in the polyoxometalate family. Further, the electrochemistry property of the compound is studied.