The reaction of either [RhCl(C8H14)(2)](2) or [RhCl(C2H4)(2)](2) with tBu(2
)PCH(2)CH(2)C(6)H(5) (3) affords at room temperature the five-coordinate ar
ylhydridorhodium(III) complex 4, the molecular structure of which has been
determined by X-ray crystallography. The C-H metalation is completely rever
sible, as is shown by the formation of trans-[RhCl(CO)(3)(2)] from 4 and CO
. Compound 4 also reacts with PhC=CH, H-2, and AgPF6 to give products 7-9 c
ontaining the intact phosphine ligand 3.