EXPERIMENTS AND STRATEGIES FOR THE ASSIGNMENT OF FULLY C-13 N-15-LABELED POLYPEPTIDES BY SOLID-STATE NMR/

High-resolution heteronuclear NMR correlation experiments and strategi es are proposed for the assignment of fully C-13/N-15-labelled polypep tides in the solid state. By the combination of intra-residue and inte r-residue C-13-N-15 correlation experiments with C-13-C-13 spin-diffus ion studies, it becomes feasible to partially assign backbone and side -chain resonances in solid proteins. The performance of sequences usin g N-15 instead of C-13 detection is evaluated regarding sensitivity an d resolution for a labelled dipeptide (L-Val-L-Phe). The techniques ar e used for a partial assignment of the N-15 and C-13 resonances in hum an ubiquitin.