Foldamers provide important insights into the fundamentals of noncovalent folding, which is of primary importance for understanding biological systems and developing novel self-assembling materials. The structure of artificial foldamers in solution has been studied using a variety of indirect spectroscopic techniques and theoretical methods. X-ray scattering using a high flux synchrotron source has been recently shown to provide a powerful means of studying small organic and biological arrays that are formed because of noncovalent self-assembly in solution but has not been applied to foldamer structures. We present small angle X-ray scattering (SAXS) studies on a m-phenylene ethynylene oligomer (mPE) in acetonitrile, providing for the first time-direct structural data on a mPE foldamer in solution.