In this paper, one supermolecular compound, namely, p-[C20H18N2O4][Mo8O26]0.5·H2O (1) has been synthesized from 1,4-bis[4-nitrile-pyridine)-N-methylene]phenyldibromide (L1) and (NH4)6Mo7- O24·4H2O by hydrothermal method. The structure has been confirmed through single-crystal X-ray diffraction analyses and further characterized by elemental analyses, IR spectra. The adsorption property of compound 1 has bee studied, Thus it’s much important to enrich the types of chemicals.