Unambiguous correlations of backbone amide and aliphatic gamma resonances in deuterated proteins

Two 3D NMR pulse sequences that correlate aliphatic gamma carbon resonance frequencies to amide proton and nitrogen chemical shifts in perdeuterated proteins are presented. The HN(CO-CACB)CG provides only interresidue connectivities (NH(i) and C gamma((i-1))) while the HN(CACB)CG detects both the inter- and intraresidue (NH(i) and C-gamma(i) or Cgamma(i-1) correlations. These two experiments are useful for sequential assignments and the identification of residue type from the C-gamma shifts. Spectra acquired on a perdeuterated 53-kDa protein illustrate the sensitivity and utility of these experiments. (C) 1998 Academic Press.