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Abstract Herein, we report the synthesis of a nitrone‐linked covalent organic framework, COF‐115, by combiningN,N′,N′,N′′′‐(ethene‐1, 1, 2, 2‐tetrayltetrakis(benzene‐4, 1‐diyl))tetrakis(hydroxylamine) and terephthaladehyde via a polycondensation reaction. The formation of the nitrone functionality was confirmed by solid‐state¹³C multi cross‐polarization magic angle spinning NMR spectroscopy of the¹³C‐isotope‐labeled COF‐115 and Fourier‐transform infrared spectroscopy. The permanent porosity of COF‐115 was evaluated through low‐pressure N₂, CO₂, and H₂sorption experiments. Water vapor and carbon dioxide sorption analysis of COF‐115 and the isoreticular imine‐linked COF indicated a superior potential ofN‐oxide‐based porous materials for atmospheric water harvesting and CO₂capture applications. Density functional theory calculations provided valuable insights into the difference between the adsorption properties of these COFs. Lastly, photoinduced rearrangement of COF‐115 to the associated amide‐linked material was successfully demonstrated.