Crystal Preparation, Scoring and Handling for time-resolved Serial Crystallography Applications

S. Botha1,2 , R. Schubert1,2, Markus Perbandt1,2, Christian Betzel1,2

1University of Hamburg, Laboratory for Structural Biology of Infection and Inflammation, c/o DESY, Build. 22a, Notkestrasse 85, 22607 Hamburg, Germany

2Center of Ultrafast Imaging, c/o DESY, Build. 99, Luruper Chaussee 149, 22761 Hamburg, Germany

Sabine.botha@uni-hamburg.de


Serial femtosecond X-ray crystallography (SFX) is a rapidly evolving new method for structure determination using thousands of microcrystals and femtosecond, highly brilliant X-ray pulses from a free-electron Laser (FEL) [1]. A single diffraction pattern is recorded per crystal in a diffraction-before-destruction approach rendering this method virtually radiation-damage free. In the past 3 years a low-dose, serial method of data collection has been adapted to synchrotron radiation use at highly brilliant micro-focus beam lines, allowing room temperature data collection with data quality sufficient for de novo phasing [2]. It has also been shown that exposure times of less than 3ms were sufficient for collecting serial room-temperature data using for example a lysozyme microcrystal suspension [3]. The ability to collect room temperature data opens up the possibility of time resolved studies, as bio-macromolecules can now be probed in their native environments.

Despite this new method of serial crystallography holding great promise for macromolecular biological studies, the major bottleneck to date is having a reliable method for determining the quality of the thousands of microcrystals. Particularly for FEL application, the crystals are often so small they do not yield determinable diffraction at a synchrotron, let alone at an in house X-ray source. To make matters worse, beam time is scarce, making it essential to reliably distinguish protein nanocrystals from amorphous precipitate and ideally even diffraction quality of the crystals prior to accessing the beam. However, measuring at room temperature and collecting a single diffraction pattern from thousands of identical crystals makes it possible to use this technique to study enzymatic reactions of proteins in substrate mixing and substrate caging approaches.

We will present various methods for reliably growing microcrystals for SFX application along with different methods for determining crystal quality in preparation for an FEL or synchrotron beam time. In addition, special attention will be paid to scoring and handling of the crystal slurries, essential for structure determination using serial crystallography techniques. And finally, preliminary results towards applying serial crystallography at synchrotrons towards time-resolved studies will be presented.

1. H. N. Chapman et al., Nature, 470, (2011), 73–77.

2. S. Botha et al., Acta Crystallogr D Biol Crystallogr., 71(Pt 2), (2015), 387-97.

3. F. Stellato et al., IUCrJ, 1(Pt 4), (2014), 204-12.