title: A time-saving strategy for MAS NMR spectroscopy by combining nonuniform sampling and paramagnetic relaxation assisted condensed data collection.
abstract: We present a time-saving strategy for acquiring 3D magic angle spinning NMR spectra for chemical shift assignments in proteins and protein assemblies in the solid state. By simultaneous application of nonuniform sampling (NUS) and paramagnetic-relaxation-assisted condensed data collection (PACC), we can attain 16-fold time reduction in the 3D experiments without sacrificing the signal-to-noise ratio or the resolution. We demonstrate that with appropriate concentration of paramagnetic dopant introduced into the sample the overwhelming majority of chemical shifts are not perturbed, with the exception of a limited number of shifts corresponding to residues located at the surface of the protein, which exhibit small perturbations. This approach enables multidimensional MAS spectroscopy in samples of intrinsically low sensitivity and/or high spectral congestion where traditional experiments fail, and is especially beneficial for structural and dynamics studies of large proteins and protein assemblies.
authors.affiliation: Department of Chemistry and Biochemistry, University of Delaware, Newark, Delaware 19716, USA.
authors.forename: Shangjin
authors.initials: S
authors.lastname: Sun
authors.forename: Si
authors.initials: S
authors.lastname: Yan
authors.forename: Changmiao
authors.initials: C
authors.lastname: Guo
authors.forename: Mingyue
authors.initials: M
authors.lastname: Li
authors.forename: Jeffrey C
authors.initials: JC
authors.lastname: Hoch
authors.forename: John C
authors.initials: JC
authors.lastname: Williams
authors.forename: Tatyana
authors.initials: T
authors.lastname: Polenova
mesh_terms: D003300:Copper / Q000737:chemistry; D003625:Data Collection / Q000379:methods*; D004492:Edetic Acid / Q000737:chemistry; D004578:Electron Spin Resonance Spectroscopy; D009682:Magnetic Resonance Spectroscopy; D013223:Statistics as Topic; D013997:Time Factors
chemical_list: D003300:Copper; D004492:Edetic Acid