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.

queen_honey_blossom answered 1 year ago

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