In a typical experimental procedure, 0.065 mmol of the [CuS t Bu]n complex was first dispersed in 1 mL of dichloromethane (DCM) to create a uniform suspension. This suspension was then treated with 0.09 mmol of CF3COOH while stirring continuously at room temperature, until the solution became transparent. Afterward, 0.065 mmol of a freshly prepared dpb linker, dissolved in 1 mL of N,Ndimethylacetamide (DMAc), was gradually added to the reaction mixture dropwise. The entire solution was allowed to stand at room temperature, undisturbed, for a period of two days to enable crystallization. At the end of this period, rod-like yellow crystals (yield: 40.6% on the basis of Cu) formed and were observed at the interface between the two immiscible liquids. The crystal morphology and chemical composition were confirmed through optical microscopy and SEM imaging combined with EDS analysis (Fig. and Fig. ).