We report what we believe to be the first experimental demonstration of nondegenerate four-wave mixing in a microstructure fiber. The effect of the chi((3)) nonlinearity is enhanced in such a fiber because of the small core area, and we achieve phase matching by operating near the zero-dispersion wavelength (?750 nm) . We have observed parametric gains of more than 13 dB in 6.1-m-long fiber with a pump peak power of only 6 W. We compare our experimental gain results with those predicted by theory and explore the effects of Raman shift and (or) amplification and cascaded nonlinear mixing.