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A novel compound [(NH4)6][Gd2Mo36O112(H2O)20]·52H2O (1) was obtained from the reaction of (NH4)6Mo7O24·4H2O with GdCl3 at pH = 1.32. The X-ray structural analysis reveals that 1 crystallizes in monoclinic system, space group C2/c, Mr = 6937.77,