A mixed‐ligand divalent coordination polymer (CP) [Cu2(muco)2(py)4]⋅4H2O⋅2EtOH (1) has been synthesized by the reaction of Cu(ClO4)2⋅6H2O and pyridine (py) with trans, trans‐muconic acid (H2muco). The compound 1 has two‐dimensional (2D) sheet structure with approximately a square‐grid network containing one‐dimensional (1D) channels. Lattice water molecules are located in the void spaces and form discrete Z‐type water tetramer cluster. Interestingly, the compound 1 formed a Schottky interface with Al material which is supported from the impedance spectroscopy (IS) based network analysis. The photosensing parameters show that the material is well responsive to the illumination with sound detectivity power and rectification ratio. Therefore, this material has potential to be used as a Schottky diode as well as a photosensing device.

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