Efficient Synthesis of Nanoscale Macrocyclic Hydrocarbons

In unusually high yields of 75 and 70% respectively, the macrocycles with six (1) and twelve arene units have been efficiently synthesized by cyclization of α‐iodo‐ω‐ethynylphenyl‐acetylene oligomers. The success is probably due to the preassembly of these difunctional building blocks. Molecular models indicate an inner diameter of 8.4 Å for 1 and 22 Å (!) for the larger macrocycle. (Figure Presented.)