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The structure of the [Rh 2 C 3 ] + ion and its reaction with CH 4 in the gas phase have been studied by infrared photodissociation spectroscopy and mass spectrometry in conjunction with quantum chemical calculations. The [Rh 2 C 3 ] + ion is characterized to have an unsymmetrical linear [Rh-C-C-C-Rh] + structure existing in two nearly isoenergetic spin states. The [Rh 2 C 3 ] + ion reacts with CH 4 at room temperature to form [Rh 2 C] + + C 3 H 4 and [Rh 2 C 2 H 2 ] + + C 2 H 2 as the major products. In addition to the [Rh 2 C] + ion, the [Rh 2  13 C] + ion is formed at about one-half of the [Rh 2 C] + intensity when the isotopic-labeled 13 CH 4 sample is used. The production of [Rh 2  13 C] + indicates that the linear C 3 moiety of [Rh 2 C 3 ] + can be replaced by the bare carbon atom of methane with all four C-H bonds being activated. The calculations suggest that the overall reactions are thermodynamically exothermic, and that the two Rh centers are the reactive sites for C-H bond activation and hydrogen atom transfer reactions.

Quadruple C–H Bond Activations of Methane by Dinuclear Rhodium Carbide Cation [Rh2C3]+

Quadruple C–H Bond Activations of Methane by Dinuclear Rhodium Carbide Cation [Rh₂C₃]⁺