TiO2- supported gold species were prepared via the deposition-precipitation route, with conservation of the initial speciation by freeze-drying. The structural and electronic properties of the Au species were investigated by X-ray absorption spectroscopy, electron microscopy, and IR spectroscopy of adsorbed CO in four states. Exclusively Au-III was deposited on the TiO2 surface in patches ranging from isolated Au ions to three-dimensional clusters. This paper illustrates in detail the unique contributions of all characterization techniques to this structural model.