A water-insoluble Keggin-type polyoxomolybdovanadate nanocluster, (Et 4 N) 4 [VMo 12 O 40 ]ÁMeCN (1) was synthesized and crystallized in acetonitrile.The catalyst was characterized by X-ray crystallography, UV-Vis, thermogravimetric analysis (TGA), cyclic voltammetry (CV), and FT-IR techniques. Degradation of organic dyes, Amido black 10B (AB10B) and Methylene blue (MB) was investigated by 1/H 2 O 2 system at room temperature and the influence of different conditions on the decomposition of AB10B and MB dyes such as catalyst dosage, oxidant concentration, pH, radical scavengers, and reusability of 1 were studied.