Synthesis, Crystal Structure, Spectroscopic and Electrochemical Properties of a Copper Coordination Polymer with Unprecedented Topology

A copper cyanide coordination polymer [Cu 8 (CN) 8 (bbtz) 2 ] n ( 1 ) [bbtz = 1,4‐bis(1,2,4‐trizal‐1‐ylmethyl)benzene] was synthesized following a synchronous redox and self‐assembly reaction under the solvothermal condition, and characterized by elemental analysis, infrared spectroscopy, and single‐crystal X‐ray diffraction. Interestingly, complex 1 exhibits a two‐dimensional conjugated pillared double‐layer architecture and an unprecedented (3,3,4)‐connected network with the point symbol (6.7.10) 2 (6.7 2 ) 2 (6 2 .7 3 .10) topology. Moreover, the thermogravimetric analysis indicates complex 1 has highly thermal stability, and the solid‐state emission spectrum for its crystalline material displays a strong green luminescence band ( λ max = 565 nm) at room temperature. The electrochemical behavior of complex 1 is determined by the scan rates in the range from –0.5 to +0.3 V at room temperature, and exhibits different redox processes.