In <i>situ</i> diffuse reflectance infrared spectroscopy of CO adsorption on reduced Ru/ZSM-5 reveals that, under appropriate conditions, in addition to the linearly adsorbed CO on metallic Ru particles (at 2045 ± 10 cm<sup>−1</sup>), two multicarbonyls involving oxidized Ru can be generated. These multicarbonyl species are characterized by IR doublets at 2080 and 2138 cm<sup>−1</sup> and at 2086 and 2150 cm<sup>−1</sup>, respectively. Direct evidence for the consumption of both types of the ZSM-5 surface hydroxyl groups (silanol and Brønsted) during the oxidative adsorption of CO has been obtained. Each of these two OH types is believed to be associated with one of the multicarbonyl species.
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