title: Structural heterogeneity in microcrystalline ubiquitin studied by solid-state NMR.
abstract: By applying [1-(13) C]- and [2-(13) C]-glucose labeling schemes to the folded globular protein ubiquitin, a strong reduction of spectral crowding and increase in resolution in solid-state NMR (ssNMR) spectra could be achieved. This allowed spectral resonance assignment in a straightforward manner and the collection of a wealth of long-range distance information. A high precision solid-state NMR structure of microcrystalline ubiquitin was calculated with a backbone rmsd of 1.57 to the X-ray structure and 1.32 Å to the solution NMR structure. Interestingly, we can resolve structural heterogeneity as the presence of three slightly different conformations. Structural heterogeneity is most significant for the loop region β1-β2 but also for β-strands β1, β2, β3, and β5 as well as for the loop connecting α1 and β3. This structural polymorphism observed in the solid-state NMR spectra coincides with regions that showed dynamics in solution NMR experiments on different timescales.
authors: Department of NMR-Based Structural Biology, Max Planck Institute for Biophysical Chemistry, Göttingen, Germany; Leibniz-Institut für Molekulare Pharmakologie, Berlin, Germany; Institut für Biologie, Humboldt-Universität, zu Berlin, Berlin, Germany.
authors: Hannes Klaus
authors: HK
authors: Fasshuber
authors: Nils-Alexander
authors: NA
authors: Lakomek
authors: Birgit
authors: B
authors: Habenstein
authors: Antoine
authors: A
authors: Loquet
authors: Chaowei
authors: C
authors: Shi
authors: Karin
authors: K
authors: Giller
authors: Sebastian
authors: S
authors: Wolff
authors: Stefan
authors: S
authors: Becker
authors: Adam
authors: A
authors: Lange
mesh_terms: D018360:Crystallography, X-Ray; D008958:Models, Molecular; D019906:Nuclear Magnetic Resonance, Biomolecular; D017510:Protein Folding; D017433:Protein Structure, Secondary; D012996:Solutions / Q000737:chemistry; D025801:Ubiquitin / Q000737:chemistry*
chemical_list: D012996:Solutions; D025801:Ubiquitin
keywords: 13C sparse labeling; dynamics; heterogeneity; solid-state NMR; ubiquitin
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