title: 13C-detected through-bond correlation experiments for protein resonance assignment by ultra-fast MAS solid-state NMR.
abstract: We present two sequences which combine ((1)H,(15)N) and ((15)N,(13)C) selective cross-polarization steps with an efficient variant of the J-based homonuclear transfer scheme, in which a spin-state-selective (S(3)E) block is incorporated to improve both resolution and sensitivity in the direct (13)C dimension. We propose these two sequences as a part of a suite of four N-C correlation experiments allowing for the assignment of protein backbone resonances in the solid state. We illustrate these experiments under ultra-fast magic angle spinning conditions on two samples of microcrystalline dimeric human superoxide dismutase (SOD, 153×2 amino acids), in its diamagnetic ("empty", Zn(II)) and paramagnetic (Cu(II), Zn(II)) states.
authors.affiliation: Centre de RMN à Très Hauts Champs, UMR 5280 CNRS/Ecole Normale Supérieure de Lyon, University of Lyon, 5 rue de la Doua, 69100 Villeurbanne (France), Fax: (+33) 04 78 89 67 61 http://www.ens-lyon.fr/crmn.
authors.forename: Emeline
authors.initials: E
authors.lastname: Barbet-Massin
authors.forename: Andrew J
authors.initials: AJ
authors.lastname: Pell
authors.forename: Michael J
authors.initials: MJ
authors.lastname: Knight
authors.forename: Amy L
authors.initials: AL
authors.lastname: Webber
authors.forename: Isabella C
authors.initials: IC
authors.lastname: Felli
authors.forename: Roberta
authors.initials: R
authors.lastname: Pierattelli
authors.forename: Lyndon
authors.initials: L
authors.lastname: Emsley
authors.forename: Anne
authors.initials: A
authors.lastname: Lesage
authors.forename: Guido
authors.initials: G
authors.lastname: Pintacuda
mesh_terms: D002247:Carbon Isotopes / Q000032:analysis*; D019906:Nuclear Magnetic Resonance, Biomolecular; D011506:Proteins / Q000737:chemistry*; D013997:Time Factors
chemical_list: D002247:Carbon Isotopes; D011506:Proteins
keywords: J-coupling; magic angle spinning; paramagnetism; solid-state nuclear magnetic resonance spectroscopy; superoxide dismutase