[2.n](2,5)Thiophenophanes (n = 3-5) having a cyclobutane ring were successf
ully synthesized by the intramolecular [2 + 2] photocycloaddition of alpha,
omega-bis(5-vinyl-2-thienyl)alkanes. The yields, conformation, and dynamic
behavior of the thiophenophanes were significantly dependent on the oligome
thylene chain length, n.