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Neutral diphenylcarbenerhodium(I) complexes of the general composition trans-[RhX(=CPh2)(PiPr3)2] (X = F (3), OCN (4), CF3CO2 (5), PhCO2 (6), CF3SO3 (7)) were prepared from the chloro or bromo precursors trans-[RhCl(=CPh2)(PiPr3)2](1) and trans-[RhBr(=CPh2)(PiPr3)2] (2) by salt metathesis in acetone and isolated in excellent yields. While treatment of 1 with Tl(acac[F6]) afforded the substitution product trans-[Rh(kappa1-acac[F6])(=CPh2)(P iPr3)2] (8), the corresponding reaction of 1 with Tl(acac) gave the chelate compound [Rh(kappa2-acac)(=CPh2)(PiPr3)] (9) with only one phosphine ligand attached to the metal center. In acetone solution, the triflato complex 7 is in equilibrium with the cation trans-[Rh{O=C(CH3)2}(=CPh2)(P iPr3)2]+ which after addition of NaBAr4F precipitates as the BAr4F salt 11. The starting material 1 as well as the bis(triphenylphosphine) and bis(triisopropylstibine) analogues 14 and 15 react with pyridine or acetonitrile in the presence of KPF6 to yield the cationic complexes trans-[Rh(py)(=CPh2)(PPh3)2]PF6 (16) and trans-[Rh(CH3CN)(=CPh2)(L)2]PF6 (L = PiPr3 (17), SbiPr3 (18)). The BAr4F salt of the cation trans-[Rh(CH3CN)(=CPh2)(SbiPr3) 2]+ (19) was characterized by X-ray crystallography. Compounds 11, 16-19 and the bis(pyridine) derivative cis-[Rh(=CPh2)(NC5H5)2(P iPr3)]PF6 (12) are the first representatives of four-coordinate cationic diphenylcarbenerhodium(I) complexes.
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Reference：
Phosphine ligand,
Chiral phosphine ligands in asymmetric synthesis. Molecular structure and absolute configuration of (1,5-cyclooctadiene)-(2S,3S)-2,3-bis(diphenylphosphino)butanerhodium(I) perchlorate tetrahydrofuran solvate