| Abstract: | Herein we present the first hexapole 9]helicene ( H9H ). Co‐catalyzed 2+2+2] cyclotrimerization of a dinaphthopyrene (DNP) functionalized alkyne provides the hexaaryl benzene precursor 2 , which is transformed into H9H via a dehydrocyclization reaction. Formation of each embedded 9]helicene involves forging of a new C?C bond, which stitches together two 4]helicene subunits of the neighboring DNP blades, reminiscent of the initial method Martin developed for the preparation of 9]helicene in the 1960s. Single‐crystal X‐ray analysis of both 2 and H9H discloses their extremely distorted and crowded structural features. Chiral resolution, optical and electronic properties of H9H are also presented. |
