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A new hetero-metallic polyoxovanadate ({Na(H2O)3}2(μ2-H2O)4{Cu(H2O)4}2[V10O28])·2H2O (1) has been isolated by refluxing a mixture containing an aqueous solution of CuCl2 and sodium meta-vanadate at acidic condition (pH ~3.4). The Infra-Red spectroscopies along with TGA and SEM analysis have been performed in order to characterize the isolated complex. Besides, the single crystal X-Ray analysis has been carried out to determine the crystal structure of 1. The crystal structure determination from the X-ray analysis reveals that the resulting POM has a 2D layer network which is produced from the interconnection of one-dimensional chains through the sodium salt of Cu(II) associated decavanadate via O atom of decavanadate with in crystallographic 'ab' plane. The complex shows good catalytic activity towards the acetylation of ortho phenylenediamine (O-PDA) and its derivatives at usual reaction conditions. [ABSTRACT FROM AUTHOR]