Band-selective 1H-13C cross-polarization in fast magic angle spinning solid-state NMR spectroscopy.
A magic angle spinning (MAS) NMR technique to transfer polarization from protons to a specific set of the (13)C spins is introduced for the study of biomolecular samples in the solid-state. Ultrafast (>60 kHz) MAS and low irradiation rf fields are used to achieve band-selective Hartmann-Hahn cross-polarization (CP) between the whole proton bath and carbons whose resonances are close to the (13)C-transmitter offset. When compared to conventional, broadband (1)H-(13)C CP, the band-selective experiment can be established without any loss of sensitivity when polarizing the aliphatic signals of a protein sample, and with a significant gain when polarizing carbonyls. This scheme can be used as a building block in 2D (13)C-(13)C homonuclear correlation experiments to obtain a faster and more sensitive characterization of biological solids.
Laage
Ségolène
S
Université de Lyon, CNRS/ENS Lyon/UCB-Lyon 1, Centre RMN à Très Hauts Champs, 5 rue de la Doua, 69100 Villeurbanne, France.
Marchetti
Alessandro
A
Sein
Julien
J
Pierattelli
Roberta
R
Sass
Hans Juergen
HJ
Grzesiek
Stephan
S
Lesage
Anne
A
Pintacuda
Guido
G
Emsley
Lyndon
L
D002244:Carbon / Q000737:chemistry; D002247:Carbon Isotopes / Q000737:chemistry*; D009682:Magnetic Resonance Spectroscopy / Q000379:methods*; D008958:Models, Molecular; D008968:Molecular Conformation; D015394:Molecular Structure; D011522:Protons; D013696:Temperature
D002247:Carbon Isotopes; D011522:Protons; D002244:Carbon