Cutting-Edge Techniques Used for the Structural Investigation of Single Crystals

Abstract

X-ray crystallography has become the leading technique for studying the structure of matter at the atomic and molecular level. Today it underpins all sciences and is widely applied in industry. It is essential in the development of new materials. The technique is very powerful, and the range of materials that can be studied expands as new technologies evolve and are applied in innovative ways to structure solution. It is now possible to record vast amounts of diffraction data in seconds electronically, whereas it took days and months by photographic methods 30 to 40 years ago. Single crystals can be created in various ways; they can be produced from compounds that are liquids or gases at room temperature, and complete molecular structures can be presented within minutes. This short review presents recent developments that are appropriate to the single-crystal x-ray studies of chemical and materials sciences.

Variation of M···H–C Interactions in Square-Planar Complexes of Nickel(II), Palladium(II), and Platinum(II) Probed by Luminescence Spectroscopy and X-ray Diffraction at Variable Pressure

“…The aim of these new high-resolution diffraction experiments was to precisely locate experimentally the positions of hydrogen (deuterium) atoms, 43 which is possible using diffractometers. 44 To be successful, this approach must be performed on highly diffracting samples, showing Bragg peaks far beyond the standard resolution of 0.77 Å, the value used in previous studies. We take advantage of the high quality of diffraction of the six compounds, whose Bragg peaks were collected up to 0.55 Å for all compounds.…”

Effect of pressure on methylated glycine derivatives: relative roles of hydrogen bonds and steric repulsion of methyl groups

“…High-pressure single-crystal X-ray diffraction studies of different types of compounds are becoming almost routine, which is shown by numerous articles containing structural data at high pressures published in the last years. Largely due to the development of X-ray diffraction instrumentation, high-pressure cells, as well as the progress achieved in data collection and processing software (Ahsbahs, 1984(Ahsbahs, , 1987(Ahsbahs, , 2004Dunstan, 1989;Dunstan & Spain, 1989;Eremets, 1996;Kuhs et al, 1996;Wilson, 1997;Katrusiak, 1999aKatrusiak, ,b, 2004aKatrusiak, ,b, 2008Dera & Katrusiak, 1999Miletich et al, 2000;Dadashev et al, 2001;Dziubek & Katrusiak, 2002;Varga et al, 2003;Angel, 2004Angel, , 2005Boehler & De Hantsetters, 2004;Budzianowski & Katrusiak, 2004;Dawson et al, 2004;Goeta & Howard, 2004;Yufit & Howard, 2005;Angel et al, 2007;Casati et al, 2007;Girard et al, 2007;Moggach et al, 2008;Yan et al, 2008;Dittrich et al, 2009;Probert et al, 2010;Angel & Finger, 2011;Periotto et al, 2011;McMahon, 2012;Ballaran et al, 2013;Howard & Probert, 2014), structural data of good quality can now be obtained even for weakly diffracting organic crystals with many atoms in the asymmetric unit and low space-group symmetry. Since the pioneering research in the 1990s to the 2000s …”

Crystal Structure of a Hidden Protein, YcaC, a Putative Cysteine Hydrolase from Pseudomonas aeruginosa, with and without an Acrylamide Adduct

“…Crystals appeared after more than 3 months and grew to maximal dimensions of 100 μm × 10 μm × 10 μm. In both cases, crystals were too small and fragile for mass spectrometric analysis, but sufficiently large for micro-focus X-ray data collection on third generation synchrotron sources [ 18 ].…”