A one-pot synthetic process was adopted here to synthesize various Cu CAMs where the crystals were obtained through liquid-liquid interfacial crystallization process (Fig. ). In each Cu CAM synthesis, the initial step involved a complexation reaction in which the [CuS t Bu]n complex was treated with CF3COOH in DCM medium. Following the complexation, a solution containing different linker molecules was added to the reaction mixture, and the system was left to undergo crystallization. To induce more variation, the solvent used to dissolve the linkers was altered, creating a separate phase from the metal complex. The resulting crystals were characterized using single-crystal Xray diffraction (SCXRD) to analyze their structural architecture.