SIGNIFICANTLY IMPROVED RESOLUTION FOR NOE CORRELATIONS FROM VALINE AND ISOLEUCINE (C-GAMMA-2) METHYL-GROUPS IN N-15,C-13-LABELED AND N-15,C-13,H-2-LABELED PROTEINS
C. Zwahlen et al., SIGNIFICANTLY IMPROVED RESOLUTION FOR NOE CORRELATIONS FROM VALINE AND ISOLEUCINE (C-GAMMA-2) METHYL-GROUPS IN N-15,C-13-LABELED AND N-15,C-13,H-2-LABELED PROTEINS, Journal of the American Chemical Society, 120(19), 1998, pp. 4825-4831
A new NMR experiment is described for recording NOEs from Val and Ile
methyl groups in N-15,C-13- labeled or methyl-protonated, N-15,C-13,H-
2-labeled proteins that offers far superior resolution than convention
al 3D C-13-edited NOESY data sets. Resolution is achieved by recording
both the C-beta and C-gamma (Val) or C-gamma 2 (Ile) chemical shifts
as well as the chemical shift of the destination proton, and a strateg
y is introduced for refocusing homonuclear carbon couplings during the
constant-time evolution of C-beta carbon magnetization. The utility o
f the method is demonstrated with applications on a 160-residue fully
protonated N-15,C-13-labeled, dNumb PTB domain-peptide complex and a m
ethyl protonated, highly deuterated N-15,C-13-labeled complex of malto
se binding protein and beta-cyclodextrin (42 kDa).