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X-ray crystallography is a technique used to reveal how the atoms of crystalline solids are arranged, relying upon the diffraction of X-ray radiation by the periodic atomic structure. Its continual development means that it remains one of the most significant techniques for determining the structure of materials and small molecules.
To understand enzymatic redox reaction mechanisms, it is important to investigate the redox behavior at the metal centers. This Protocol describes metalloenzyme attachment to electrodes and how to perform X-ray absorption spectroelectrochemistry.
The surface features of nanoparticle catalysts change during a reaction. This protocol describes how to measure these changes in operando (in flowing liquid or gas) by X-ray photoelectron spectrometry using a modified Si3N4 window.
Crystal structure predictions have proposed the existence of polymeric H2CO3, but its high-pressure polymorphism has yet to be confirmed experimentally. Here, the authors synthesized single crystals of polymeric H2CO3 in a diamond anvil cell and demonstrated that its structure consists of polymerized \({[{{\rm{CO}}}_{4}]}^{4-}\) tetrahedra forming chains along the c-axis.
Spin-active materials with sensitive electron spin centers have drawn significant attention in quantum sensing due to their unique quantum characteristics. Herein, the authors report a molecular spin sensor based on metallofullerene Y2@C79N for in-situ monitoring of crystallization behavior and phase transitions in aromatic materials with high precision.
X-ray diffraction analysis typically affords the static 3D structures of given compounds or materials, but to understand chemical processes, the visualization of fast structural changes is desirable. Time-resolved femtosecond crystallography has now been used to monitor the structural dynamics of a photoactive metal–organic framework.
The Lewis acidity of trihaloboranes has now also been observed for tetrahalodiboranes, which bind halides to give hexahalodiborates — a new anion class.
X-ray diffraction not only paints a picture of atomic structure but also, when performed at multiple wavelengths, tells us about relative redox levels of metals in clusters.
