A highly porous 4,4-paddlewheel-connected NbO-type metal–organic framework (HNUST-2, HNUST represents Hunan University of Science and Technology) has been designed and synthesized by self-assembling [Cu2(COO)4] SBUs with a nanosized tetracarboxylate ligand prolonged by alkyne groups, 5,5′-(naphthalene-1,4-diylbis(ethyne-2,1-diyl))diisophthalic acid (H4NDED). HNUST-2 exhibits high structural stability, a porous non-interpenetration framework with open metal sites and excellent gas-uptake capacity. This MOF material possesses a high BET surface area of 2366 m2 g−1, a large unsaturated excess and total H2 uptake of 4.57 wt% and 5. 20 wt% at 20 bar and 77 K, respectively. Meanwhile, HNUST-2 also exhibits an excellent adsorption capacity for CO2 (18.07 mmol g−1 at 20 bar and 298 K) and CH4 (85.6 cm3 cm−3 at 20 bar and 298 K) with a high selectivity for CO2 over N2 (22.9) and CH4 (4.9) at 298 K.
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