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Metal–organic frameworks bearing coordinatively unsaturated Mg( ii ) sites are promising materials for gas storage, chemical separations, and drug delivery due to their low molecular weights and lack of toxicity. However, there remains a limited number of such MOFs reported in the literature. Herein, we investigate the gas sorption properties of the understudied framework Mg 2 ( m -dobdc) (dobdc 4− = 4,6-dioxido-1,3-benzenedicarboxylate) synthesized under both solvothermal and mechanochemical conditions. Both materials are found to be permanently porous, as confirmed by 77 K N 2 adsorption measurements. In particular, Mg 2 ( m -dobdc) synthesized under mechanochemical conditions using exogenous organic base displays one of the highest capacities reported to date (6.14 mmol g −1 ) for CO 2 capture in a porous solid under simulated coal flue gas conditions (150 mbar, 40 °C). As such, mechanochemically synthesized Mg 2 ( m -dobdc) represents a promising new framework for applications requiring high gas adsorption capacities in a porous solid.