Intercalation, exfoliation, and reduction of VOPO 4 ·2H 2 O were conducted in 2-butanol alone and in a mixed alcohol solvent (2-butanol and ethanol). While both processes produced crystallites of pure VOHPO 4 ·0.5H 2 O, much smaller and thinner crystallites (av. 340 nm × 35 nm) were formed in the mixed alcohol compared with 2-butanol alone (av. 950 nm × 200 nm).The small, thin crystallites of precursor VOHPO 4 ·0.5H 2 O could be transformed into sharply angular nano-sized crystallites (60 nm in length and 31 nm in thickness) of highly crystalline (VO) 2 P 2 O 7 , without mesopores. When used as a catalyst, this compound exhibited higher activity and selectivity to maleic anhydride (75% at 80% conversion) for selective oxidation of n-butane than that derived from the precursor prepared in 2-butanol alone. The high activity of the nano-sized crystallites of (VO) 2 P 2 O 7 is attributed to their large surface area (40 m 2 g -1 ), which is due to their smaller dimensions, and their high selectivity may be attributed to the lack of mesopores as well as their highly crystalline state.