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The manuscript reports the synthesis, characterization, and analysis of electronic structure in a series of complexes of small perfluorocarbon ligands with the (PNP)Rh fragment (where PNP is a diarylamido/bis(phosphine) pincer ligand). Reactions of (PNP)Rh(TBE) as the source of (PNP)Rh with CHF 3 and C 2 HF 5 produced perfluoroalkylidene complexes (PNP)Rh[double bond, length as m-dash]CF 2 and (PNP)Rh[double bond, length as m-dash]C(F)(CF 3 ). (PNP)Rh[double bond, length as m-dash]CF 2 could also be obtained via the reaction of (PNP)Rh(TBE) with Me 3 SiCF 3 /CsF, with an admixture of (PNP)Rh(C 2 F 4 ), where TBE = tert -butylethylene. Abstraction of fluoride from these neutral (PNP)RhC  x  F  y  complexes was successful, although only abstraction from (PNP)Rh[double bond, length as m-dash]CF 2 allowed unambiguous identification of the Rh product, [(PNP)Rh[triple bond, length as m-dash]CF] + . DFT computational studies allowed comparison of relative energies of (PNP)Rh(C 2 F 4 ) and [(PNP)Rh(C 2 F 3 )] + isomers as well as comparisons between the electronic structure of the [double bond, length as m-dash]CF 2 , C 2 F 4 , and [triple bond, length as m-dash]CF + complexes and their hydrocarbon analogues.

Fluorocarbene, fluoroolefin, and fluorocarbyne complexes of Rh