Novel tungsten, molybdenum, and vanadium oxides containing surfactant ions

Hydrothermal reaction of tungstic acid, molybdic acid, and vanadium pentoxide with the surfactant template dodecyltrimethylammonium bromide (DTABr) yielded one compound with a keggin, type structure, [C12H25N(CH3)(3)](6)(H2W12O40). xH(2)O, and two new layered compounds, [C12H25N(CH3)](0.5)(MoO3.25) and [C12H25N(CH3)(3)]2/3V2O5.33. H2O. The tungsten salt produced needlelike crystals of a hexagonal shape while the molybdenum and vanadium materials containing Keggin anions. The X-ray powder diffraction data of this material were indexed to a monoclinic cell with a = 50.56(4) Angstrom, b = 54.41(4) Angstrom, c = 13.12(1) Angstrom, and beta = 99.21 degrees. The observed reflections are consistent with space group C2/m. Diffraction data obtained from the molybdenum salt showed a between layerd spacing of ca. 22 Angstrom. The vanadium sale was indexed to a triclinic cell with a = 9.813(3) Angstrom, b = 11.512(3) Angstrom, c = 21.725(5) Angstrom, alpha = 95.30(1)degrees, beta = 93.82(6)degrees, and gamma = 101.12(8)degrees, with a layer spacing of 21.6 Angstrom.