title: Observing the overall rocking motion of a protein in a crystal.
abstract: The large majority of three-dimensional structures of biological macromolecules have been determined by X-ray diffraction of crystalline samples. High-resolution structure determination crucially depends on the homogeneity of the protein crystal. Overall 'rocking' motion of molecules in the crystal is expected to influence diffraction quality, and such motion may therefore affect the process of solving crystal structures. Yet, so far overall molecular motion has not directly been observed in protein crystals, and the timescale of such dynamics remains unclear. Here we use solid-state NMR, X-ray diffraction methods and μs-long molecular dynamics simulations to directly characterize the rigid-body motion of a protein in different crystal forms. For ubiquitin crystals investigated in this study we determine the range of possible correlation times of rocking motion, 0.1-100 μs. The amplitude of rocking varies from one crystal form to another and is correlated with the resolution obtainable in X-ray diffraction experiments.
authors.affiliation: Université Grenoble Alpes, IBS, F-38044 Grenoble, France.|CEA, Institut de Biologie Structurale, F-38044 Grenoble, France.|CNRS, Institut de Biologie Structurale, F-38044 Grenoble, France.
authors.forename: Peixiang
authors.initials: P
authors.lastname: Ma
authors.affiliation: Department of Chemistry, Purdue University, West Lafayette, Indiana 47907, USA.
authors.forename: Yi
authors.initials: Y
authors.lastname: Xue
authors.affiliation: Université Grenoble Alpes, IBS, F-38044 Grenoble, France.|CEA, Institut de Biologie Structurale, F-38044 Grenoble, France.|CNRS, Institut de Biologie Structurale, F-38044 Grenoble, France.
authors.forename: Nicolas
authors.initials: N
authors.lastname: Coquelle
authors.affiliation: Université Grenoble Alpes, IBS, F-38044 Grenoble, France.|CEA, Institut de Biologie Structurale, F-38044 Grenoble, France.|CNRS, Institut de Biologie Structurale, F-38044 Grenoble, France.
authors.forename: Jens D
authors.initials: JD
authors.lastname: Haller
authors.affiliation: Department of Chemistry, Purdue University, West Lafayette, Indiana 47907, USA.
authors.forename: Tairan
authors.initials: T
authors.lastname: Yuwen
authors.affiliation: Université Grenoble Alpes, IBS, F-38044 Grenoble, France.|CEA, Institut de Biologie Structurale, F-38044 Grenoble, France.|CNRS, Institut de Biologie Structurale, F-38044 Grenoble, France.
authors.forename: Isabel
authors.initials: I
authors.lastname: Ayala
authors.affiliation: Department of Chemistry, Purdue University, West Lafayette, Indiana 47907, USA.
authors.forename: Oleg
authors.initials: O
authors.lastname: Mikhailovskii
authors.affiliation: CEA, Institut de Biologie Structurale, F-38044 Grenoble, France.|Institut fu¨r Physikalische Biologie, Heinrich-Heine-Universität Düsseldorf, 40225 Düsseldorf, Germany.|ICS-6: Structural Biochemistry, Forschungszentrum Jülich, 52425 Jülich, Germany.
authors.forename: Dieter
authors.initials: D
authors.lastname: Willbold
authors.affiliation: Université Grenoble Alpes, IBS, F-38044 Grenoble, France.|CEA, Institut de Biologie Structurale, F-38044 Grenoble, France.|CNRS, Institut de Biologie Structurale, F-38044 Grenoble, France.
authors.forename: Jacques-Philippe
authors.initials: JP
authors.lastname: Colletier
authors.affiliation: Department of Chemistry, Purdue University, West Lafayette, Indiana 47907, USA.|Laboratory of Biomolecular NMR, St. Petersburg State University, St. Petersburg 199034, Russia.
authors.forename: Nikolai R
authors.initials: NR
authors.lastname: Skrynnikov
authors.affiliation: Université Grenoble Alpes, IBS, F-38044 Grenoble, France.|CEA, Institut de Biologie Structurale, F-38044 Grenoble, France.|CNRS, Institut de Biologie Structurale, F-38044 Grenoble, France.
authors.forename: Paul
authors.initials: P
authors.lastname: Schanda
mesh_terms: D003460:Crystallization; D018360:Crystallography, X-Ray; D056004:Molecular Dynamics Simulation; D009038:Motion; D019906:Nuclear Magnetic Resonance, Biomolecular; D011092:Polyethylene Glycols; D011487:Protein Conformation; D025801:Ubiquitin / Q000737:chemistry / Q000378:metabolism*
chemical_list: D025801:Ubiquitin; D011092:Polyethylene Glycols