A large-pore version of Mg-CUK-1, a water-stable metal−organic framework (MOF) with 1-D channels, was synthesized in basic water. Mg-CUK-1L has a BET surface area of 2896 m 2 g −1 and shows stark selectivity for CO 2 sorption over N 2 , O 2 , H 2 , and CH 4 . It displays reversible, multistep gated sorption of CO 2 below 0.33 atm. The dehydrated single-crystal structure of Mg-CUK-1L confirms retention of the open-channel structure. The MOF can be loaded with organic molecules by immersion in hot melts, providing single crystals suitable for X-ray diffraction. trans-Azobenzene fills the channels in a 2 × 2 arrangement. Solid-state UV−vis spectroscopy reveals that azobenzene molecules undergo reversible trans−cis isomerization, despite being close-packed; this surprising result is confirmed by DFT-simulated UV−vis spectra.
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