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In: Chemistry

Vaska’s complex is well known for its ability to bind O2 reversibly. How could you use...

Vaska’s complex is well known for its ability to bind O2 reversibly. How could you use NMR to confirm you had the complex with the requisite trans triphenylphosphine ligands?

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Expert Solution

Vaska's complex is the trivial name for the chemical compound trans-carbonylchlorobis (triphenylphosphine) iridium(I), which has the formula IrCl(CO)[P(C6H5)3]2. This square planar diamagnetic organometallic complex consists of a central iridium atom bound to two mutually trans triphenylphosphine ligands, carbon monoxide, and a chloride ion. Vaska's complex can undergo oxidative addition and is notable for its ability to bind to O2 reversibly. It is a bright yellow crystalline solid.

The synthesis involves heating virtually any iridium chloride salt with triphenylphosphine and a carbon monoxide source. The most popular method uses dimethylformamide (DMF) as a solvent, and sometimes aniline is added to accelerate the reaction. Another popular solvent is 2-methoxyethanol. The reaction is typically conducted under nitrogen. In the synthesis, triphenylphosphine serves as both a ligand and a reductant, and the carbonyl ligand is derived by decomposition of dimethylformamide, probably via a deinsertion of an intermediate Ir-C(O)H species. The following is a possible balanced equation for this complicated reaction.[2]

IrCl3(H2O)3 + 3 P(C6H5)3 + HCON(CH3)2 + C6H5NH2→ IrCl(CO)[P(C6H5)3]2 + [(CH3)2NH2]Cl + OP(C6H5)3+ [C6H5NH3]Cl + 2 H2O

Typical sources of iridium used in this preparation are IrCl3·xH2O and H2IrCl6.


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