Cyclophane chemistry has contributed greatly to the understanding of fields as varied as molecular and cationic recognition to fundamental principles of NMR. 2 To date, the largest all-carbon [n. n] metacyclophane prepared is [5.5] metacyclophane, which was synthesized by the acid-catalyzed dimerization of δ-2-methoxyphenylvaleric acid, yet no conformational information is available about this system. 3[4.4] Metacyclophane has been prepared by a ...