title: Combining multinuclear high-resolution solid-state MAS NMR and computational methods for resonance assignment of glutathione tripeptide.
abstract: We present a complete set of experimental approaches for the NMR assignment of powdered tripeptide glutathione at natural isotopic abundance, based on J-coupling and dipolar NMR techniques combined with (1)H CRAMPS decoupling. To fully assign the spectra, two-dimensional (2D) high-resolution methods, such as (1)H-(13)C INEPT-HSQC/PRESTO heteronuclear correlations (HETCOR), (1)H-(1)H double-quantum (DQ), and (1)H-(14)N D-HMQC correlation experiments, have been used. To support the interpretation of the experimental data, periodic density functional theory calculations together with the GIPAW approach have been used to calculate the (1)H and (13)C chemical shifts. It is found that the shifts calculated with two popular plane wave codes (CASTEP and Quantum ESPRESSO) are in excellent agreement with the experimental results.
authors.affiliation: Department of Chemistry, CICECO, University of Aveiro, P-3810-193 Aveiro, Portugal.
authors.forename: Mariana
authors.initials: M
authors.lastname: Sardo
authors.forename: Renée
authors.initials: R
authors.lastname: Siegel
authors.forename: Sérgio M
authors.initials: SM
authors.lastname: Santos
authors.forename: João
authors.initials: J
authors.lastname: Rocha
authors.forename: José R B
authors.initials: JR
authors.lastname: Gomes
authors.forename: Luis
authors.initials: L
authors.lastname: Mafra
mesh_terms: D005978:Glutathione / Q000737:chemistry*; D008958:Models, Molecular; D019906:Nuclear Magnetic Resonance, Biomolecular; D009842:Oligopeptides / Q000737:chemistry*; D011789:Quantum Theory
chemical_list: D009842:Oligopeptides; D005978:Glutathione