Abstract: | We have successfully designed and synthesized a new tetracarboxylic linker, which constructed its first three‐dimensional microporous metal‐organic framework (MOF ), [Cu2(DDPD )(H2O )2]•Gx ( ZJU ‐13 , H4DDPD =5,5'‐(2,6‐dihydroxynaphthalene‐1,5‐diyl)diisophthalic acid, ZJU =Zhejiang University, G = guest molecules) via solvothermal reaction. Due to open Cu2+ sites and optimized pore size, the activated ZJU ‐13a displays high separation selectivity for C2H2 /CH4 of 74 and C2H2 /CO2 of 12.5 at low pressure by using Ideal Adsorbed Solution Theory (IAST ) simulation at room temperature. |