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Metal-organic frameworks (MOFs) are promising gas adsorbents. Knowledge of the behavior of gas molecules adsorbed inside MOFs is crucial for advancing MOFs as gas capture materials. However, their behavior is not always well understood. In this work, carbon dioxide (CO 2 ) adsorption in the microporous α-Zn 3 (HCOO) 6 MOF was investigated. The behavior of the CO 2 molecules inside the MOF was comprehensively studied by a combination of single-crystal X-ray diffraction (SCXRD) and multinuclear solid-state magnetic resonance spectroscopy. The locations of CO 2 molecules adsorbed inside the channels of the framework were accurately determined using SCXRD, and the framework hydrogens from the formate linkers were found to act as adsorption sites. 67 Zn solid-state NMR (SSNMR) results suggest that CO 2 adsorption does not significantly affect the metal center environment. Variable-temperature 13 C SSNMR experiments were performed to quantitatively examine guest dynamics. The results indicate that CO 2 molecules adsorbed inside the MOF channel undergo two types of anisotropic motions: a localized rotation (or wobbling) upon the adsorption site and a twofold hopping between adjacent sites located along the MOF channel. Interestingly, 13 C SSNMR spectroscopy targeting adsorbed CO 2 reveals negative thermal expansion (NTE) of the framework as the temperature rose past ca. 293 K. A comparative study shows that carbon monoxide (CO) adsorption does not induce framework shrinkage at high temperatures, suggesting that the NTE effect is guest-specific.

Exploring Host–Guest Interactions in the α-Zn3(HCOO)6 Metal-Organic Framework

Exploring Host–Guest Interactions in the α-Zn₃(HCOO)₆ Metal-Organic Framework