Fast Resonance Assignment and Fold Determination of Human Superoxide Dismutase by High‐Resolution Proton‐Detected Solid‐State MAS NMR Spectroscopy

Re-protonation is key: A combination of a high magnetic field (1 GHz) and ultra-fast magic-angle spinning (60 kHz) allows easy detection of NMR spectra revealing details of secondary and tertiary structures of medium-sized proteins. The technique was applied to the 153-residue microcrystalline ZnII-loaded superoxide dismutase (ZnII-SOD) fully [2H,13C,15N]-labeled and 100 % re-protonated at the exchangeable sites.