An improved synthetic pathway for trans-4,4′-azo-1,2,4-triazole (atrz) was discovered. Pure atrz was obtained directly without any other separation step in an environment friendly process. Treatment of atrz with zinc perchlorate and cupric nitrate led to the isolation of {[Zn(μ-atrz) 3 ](ClO 4 ) 2 ·2H 2 O} n and {[Cu(μ-atrz) 3 ](NO 3 ) 2 ·2H 2 O} n , which were well characterized. Their structures were determined by X-ray crystallographic analysis. The calculation results of the formation of {[Zn(μ-atrz) 3 ](ClO 4 ) 2 2H 2 O} n and {[Cu(μ-atrz) 3 ](NO 3 ) 2 2H 2 O} n indicates that the perfect crystal structures in spite of much resistance. A fundamental understanding of the structure and thermal properties involves factors, such as conjugated system, crystal structure, and inorganic metallic compounds that affect their thermal behavior. The high energy of the coordination compounds consists of chemical, electronic, and potential energy. The potential for the improvement of the coordination polymer opens up a new world for research of energetic materials.

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