N,N’‐Dipyrid‐3‐yl‐1,4,5,8‐naphthalenediimide linked to two tris(pentafluorophenyl)borane (1) exhibits strong fluorescence emission in the solid state by the formation of a charge‐transfer complex containing small aromatic guest molecules. Hydrophobic 1 was dissolved in water by mixing with poly‐L‐lysine (PLL) as a solubilizing agent. The 1‐PLL complex could include small aromatic guest molecules in water, significantly increasing the fluorescence. The fluorescence maxima of 1 in aqueous solution and solid state were different depending on the guest molecule. Therefore, compound 1 was prepared as aqueous solution with information of fluorescence on solids by complexation with PLL.

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