Nickel-mediated synthesis of [9]cycloparaphenylene ([9]CPP) is described. L-shaped diphenylcyclohexane monomers underwent cyclotrimerization under the influence of [Ni(cod)2]/bipy. X-ray crystal-structure analysis and VT NMR analysis of the thus-formed cyclic trimer confirmed its triangle structure and interesting cyclohexane-flipping behavior in solution. Cyclic trimer was converted to [9]CPP by acid-mediated aromatization. The first X-ray crystal structure of [9]CPP is also described.
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