A 2-fold interpenetrating 3D pillar-layered MOF, which was assembled from a mixed-linker and paddle-wheel cluster, was successfully synthesized. It possesses good thermal and water stability as well as high selectivity for C2H6 over CH4 and CO2 over N2 under ambient conditions, which was further proved by breakthrough experiments. Moreover, this porous material exhibits good detection of Cu2+, [Co(NH3)6]3+ and Fe3+ in an aqueous solution.