A hexaazatriphenylene (HAT) derivative (compound 1) that bears four n-octyl chains and two thienyl groups was designed and synthesized. Further light-induced oxidation coupling reaction led to thienyl-fused compound 2. Their photophysical and electrochemical properties and self-assembly behavior have been investigated by UV/Vis, fluorescence, and (1)H NMR spectroscopies, cyclic voltammetry (CV), scanning electron microscopy (SEM), and powder X-ray diffraction (PXRD). Although the difference in compounds 1 and 2 only lie in one single bond that connects the two thienyl segments, they displayed remarkably different properties, revealing an interesting structure-property relationship.
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