A new fluorocarbon-chain-containing molecule, CF3(CF2)(7)C(O)N(H)CH2CH2SH, for self-assembly was synthesized using a simple and general technique. Self-assembled monolayers of this molecule were studied using ellipsometry, contact angle measurements, grazing-incidence infrared spectroscopy, X-ray photoelectron spectroscopy, and near-edge X-ray absorption fine structure measurements. The films were found to be uniform and reproducible, presenting a fluorocarbon surface (theta(adv)(H2O) = 114 degrees) with predominantly CF3 groups exposed. The C=O and N-H dipoles are found to be oriented parallel to the gold surface, with the fluorocarbon axis oriented perpendicular to the surface.