To develop efficient adsorbent materials for C2Hx, separation from methane, herein, we design a new 3-D framework (NbU-5) using the pore space partition strategy: Zn-2(O2CR)(4) paddlewheel units connect tetra-carboxylic linkers to build a primary framework, and 4,4-bipyridine, which acts as a pore-partitioning agent, has been successfully inserted into the cage of the primary framework. Remarkably, NbU-5 exhibits excellent C2H2/CH4 and C2H6/CH4 selectivity, which is proved by breakthrough experiments.