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The separation of ethane from its corresponding ethylene is an important, challenging, and energy-intensive process in the chemical industry. Here we report a microporous metal-organic framework, iron(III) peroxide 2,5-dioxido-1,4-benzenedicarboxylate [Fe₂(O₂)(dobdc) (dobdc⁴⁻: 2,5-dioxido-1,4-benzenedicarboxylate)], with iron (Fe)–peroxo sites for the preferential binding of ethane over ethylene and thus highly selective separation of C₂H₆/C₂H₄. Neutron powder diffraction studies and theoretical calculations demonstrate the key role of Fe-peroxo sites for the recognition of ethane. The high performance of Fe₂(O₂)(dobdc) for the ethane/ethylene separation has been validated by gas sorption isotherms, ideal adsorbed solution theory calculations, and simulated and experimental breakthrough curves. Through a fixed-bed column packed with this porous material, polymer-grade ethylene (99.99% pure) can be …