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A highly crystalline perylene imide supramolecular photocatalyst (PDI‐NH) is synthesized via imidazole solvent method. The catalyst shows a breakthrough oxygen evolution rate (40.6 mmol g−1 h−1) with apparent quantum yield of 10.4% at 400 nm, which is 1353 times higher than the low crystalline PDI‐NH. The highly crystalline structure comes from the ordered self‐assembly process in molten imidazole...