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The reactivity of the {RhNO} 9 complex [Rh(PCP  Bu)(NO)]˙ (1˙) with NO˙ was studied. A disproportionation reaction takes place in which N 2 O is released quantitatively, while the complex Rh(PCP  Bu)(NO)(NO 2 ) (2), with coordinated nitrite, is formed. The new complex 2 was fully characterized by multinuclear NMR techniques, IR and X-ray diffraction. The X-ray structure reveals a square pyramidal geometry with an N-bound nitro ligand trans to the C ipso of the PCP ligand and a bent nitrosyl ligand in the apical position. IR measurement of released N 2 O confirms that one equivalent forms for each molecule of 1˙. Infrared spectroscopic experiments with 1˙- 15 NO and 14 NO˙ suggest that the reaction occurs through the intermediacy of a dinitrosyl complex. In addition, DFT calculations were performed to provide more evidence on the structure of the intermediates and to support the observed reactivity.

NO˙ disproportionation by a {RhNO}9pincer-type complex

NO˙ disproportionation by a {RhNO}⁹pincer-type complex