Both the cubic and orthorhombic ZrW0.8Mo1.2O8 were prepared by precursor-microwave route. The cubic phase belonged to a-ZrW2O8 structure type and the orthorhombic phase was refined with the structural model of LT-ZrMo2O8 by the Rietveld method. The orthorhombic phase belonged to Pmn21 space group and the cell parameters were ao=0.597 1(9) nm, bo=0.730 6(1) nm, co=0.912 7(1) nm, Rp%=9.37; wRp%=11.81. The TEM images were also given. The comparison was made between precursor-heated and precursor-microwave routes. Metastable polymorphic phase was favorably formed by the latter method.
