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Gold clusters stabilized by chemisorbed monolayers of octane-, dodecane-or hexadecanethiolate have been investigated in solution and in the solid phase. These materials can be pumped free of solvent to form a dark brown solid that can be re-dissolved in nonpolar solvents. Their exceptional stability suggests they be viewed as cluster compounds. The self-assembled alkanethiolate monolayers stabilizing the metal clusters can be investigated using techniques that are insufficiently sensitive for study of a monolayer on a flat surface, eg „'H and 13C NMR, elemental analysis, differential scanning calorimetry (DSC), thermogravimetry (TGA), and diffusion-ordered NMR spectroscopy (DOSY). Results from such measurements, combined with small-angle X-ray scattering (SAXS) data on solutions of the clusters and images from scanning tunneling (STM), and atomic force microscopy (AFM), are consistent with a small …