Effective from 2021B, CryoTEM will be offered in addition to SPring-8 public beamlines for protein crystallography and BioSAXS beamlines. Two CryoTEMs, EM01CT(JEOL CRYO ARM 300), and EM02CT(JEOL CRYO ARM 200)are provided as auxiliary instruments for evaluating the properties of samples for crystallization, such as monodispersity and structural heterogeneity.
In March 2018, KEK obtained a 200 kV cryogenic electron microscopy(cryo-EM; a Talos Arctica G2 with a Falcon 3EC direct electron detector)and prepared a pipeline for solving high-resolution structures of macromolecular biomolecules, such as proteins, DNA, and RNA. In October 2018, the cryo-EM facility in KEK opened to academic and industrial users. Our mission is three-fold:to provide cryo-EM machine time for external users, to support grid-prep and data collection(and single particle analysis, if needed), and to help users acquire cryo-EM skills. One remarkable result is the single-particle analysis of an 860-kDa enzyme at 2.05 angstrom resolution, which suggested that we had established a proper protocol for cryo-EM operation and single-particle analysis. We will continue to support external users and carry out cryo-EM single particle analysis of macromolecular biomolecules.
In general, the X-ray crystal structure analysis of synthetic polymers cannot necessarily lead us to the satisfactorily correct answer because of the low quality of the diffraction data due to the small crystallite size, making the discussion of the structure-property relationship quite ambiguous. The harmonic combination of X-ray and neutron diffraction data analyses increases the reliability of the derived crystal structures. The actual examples are introduced about the crystal structures of atactic-poly(vinyl alcohol) and its iodine complex to demonstrate the powerfulness of the idea of coupling the different types of diffraction data.
Li superionic conductor such as Li10GeP2S12 is expected for its application as solid electrolyte in all-solid-state lithium-ion secondary battery, which has potential to improve the operational temperature range and rate characteristic, in comparison with conventional battery. As a result, there has been a growing interest for basic understanding of the conduction mechanism in Li-superionic conductors. We investigated Li10GeP2S12 based on syntheses of large single crystals, low-temperature single crystal neutron diffraction experiments, AC impedance measurements using single crystals and first-principles calculations. Consequently, we found that a correlated migration of Li ions governs the overall Li-ion conduction in Li10GeP2S12.
We developed the spin-contrast-variation neutron powder diffractometry to observe hydrogen atoms in a crystalline sample by polarized neutrons and by polarized protons in the crystal. With L-glutamic acid crystals dispersed in a deuterated polystyrene matrix containing a polarizing agent, we observed the intensities of the sample's diffraction peaks changing differently in accordance with the proton polarization. Diffraction peaks from hydrogen atoms can be extracted the spin-contrast-variation neutron powder diffractometry thanks to the variation of peak intensities as a function of proton polarization. This technique is expected to establish the method of analyzing structures of hydrogen-containing materials that are difficult to determine with conventional powder diffractometry.
Monitoring chemical reactions between solid and gas is important not only in general chemistry but also in industrial applications. Ceria (CeO2) is a well-known material used in various industrial and environmental applications. Ceria was kinetically reduced in hydrogen depending on the isothermal holding time at high temperature. Neutron powder diffraction analysis revealed that ceria transformed into the oxyhydroxide structure CeO2Hy(0 ≤ y ≤ 1) by hydrogen treatment. Due to detection of the vibrational modes of both OH and CeH functional groups by inelastic neutron scattering measurements, the CeH functional group was revealed to possibly exist in ceria as an aperiodic structure.