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The development of ethane (C2H6)‐selective adsorbents for ethylene (C2H4) purification, although challenging, is of prime industrial importance. Pillared‐layer metal‐organic frameworks (MOFs) possess facilely tunable pore structure and functionality, which means they have excellent potential for high‐performance C2H6/C2H4 separation applications. Herein, we report a family of isostructural pillared‐layer...