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A series of perylene bisimide (PBI) dyes bearing various aryl substituents in 1,6,7,12 bay positions has been synthesized by Suzuki cross‐coupling reaction. These molecules exhibit an exceptionally large and conformationally fixed twist angle of the PBI π‐core due to the high steric congestion imparted by the aryl substituents in bay positions. Single crystal X‐ray analyses of phenyl‐, naphthyl‐ and...