Christian G Roessler1, Rakhi Agarwal2, Marc Allaire3, Roberto Alonso-Mori4, Babak Andi1, José F R Bachega5, Martin Bommer6, Aaron S Brewster7, Michael C Browne4, Ruchira Chatterjee7, Eunsun Cho8, Aina E Cohen9, Matthew Cowan1, Sammy Datwani10, Victor L Davidson11, Jim Defever4, Brent Eaton10, Richard Ellson10, Yiping Feng4, Lucien P Ghislain10, James M Glownia4, Guangye Han7, Johan Hattne7, Julia Hellmich12, Annie Héroux1, Mohamed Ibrahim6, Jan Kern13, Anthony Kuczewski1, Henrik T Lemke4, Pinghua Liu8, Lars Majlof10, William M McClintock10, Stuart Myers1, Silke Nelsen4, Joe Olechno10, Allen M Orville14, Nicholas K Sauter7, Alexei S Soares15, S Michael Soltis9, Heng Song8, Richard G Stearns10, Rosalie Tran7, Yingssu Tsai16, Monarin Uervirojnangkoorn7, Carrie M Wilmot17, Vittal Yachandra7, Junko Yano7, Erik T Yukl17, Diling Zhu4, Athina Zouni6. 1. Photon Sciences Division, Brookhaven National Laboratory, Upton, NY 11973-5000, USA. 2. Biosciences Department, Brookhaven National Laboratory, Upton, NY 11973-5000, USA. 3. Photon Sciences Division, Brookhaven National Laboratory, Upton, NY 11973-5000, USA. Electronic address: mallaire@lbl.gov. 4. Linac Coherent Light Source, SLAC National Accelerator Laboratory, Menlo Park, CA 94025, USA. 5. Centro de Biotecnologia Molecular Estrutural, Instituto de Física de São Carlos, Universidade de São Paulo, Caixa Postal 369, São Carlos, CEP: 13560-970, Brazil. 6. Institut für Biologie, Humboldt-Universität zu Berlin, D-10099 Berlin, Germany. 7. Physical Biosciences Division, Lawrence Berkeley National Laboratory, Berkeley, CA 94720-8177, USA. 8. Department of Chemistry, Boston University, Boston, MA 02215-2521, USA. 9. Stanford Synchrotron Radiation Lightsource, SLAC National Accelerator Laboratory, Menlo Park, CA 94025, USA. 10. Labcyte Inc., Sunnyvale, CA 94089, USA. 11. Burnett School of Biomedical Sciences, University of Central Florida, Orlando, FL 32816-2364, USA. 12. Max-Volmer-Laboratorium für Biophysikalische Chemie, Technische Universität, D-10623 Berlin, Germany; Institut für Biologie, Humboldt-Universität zu Berlin, D-10099 Berlin, Germany. 13. Physical Biosciences Division, Lawrence Berkeley National Laboratory, Berkeley, CA 94720-8177, USA; Linac Coherent Light Source, SLAC National Accelerator Laboratory, Menlo Park, CA 94025, USA. 14. Photon Sciences Division, Brookhaven National Laboratory, Upton, NY 11973-5000, USA; Biosciences Department, Brookhaven National Laboratory, Upton, NY 11973-5000, USA. Electronic address: allen.orville@diamond.ac.uk. 15. Photon Sciences Division, Brookhaven National Laboratory, Upton, NY 11973-5000, USA. Electronic address: soares@bnl.gov. 16. Linac Coherent Light Source, SLAC National Accelerator Laboratory, Menlo Park, CA 94025, USA; Department of Chemistry, Stanford University, Stanford, CA 94305-4401, USA. 17. Department of Biochemistry, Molecular Biology & Biophysics, University of Minnesota, Minneapolis, MN 55455, USA.
Abstract
X-ray free-electron lasers (XFELs) provide very intense X-ray pulses suitable for macromolecular crystallography. Each X-ray pulse typically lasts for tens of femtoseconds and the interval between pulses is many orders of magnitude longer. Here we describe two novel acoustic injection systems that use focused sound waves to eject picoliter to nanoliter crystal-containing droplets out of microplates and into the X-ray pulse from which diffraction data are collected. The on-demand droplet delivery is synchronized to the XFEL pulse scheme, resulting in X-ray pulses intersecting up to 88% of the droplets. We tested several types of samples in a range of crystallization conditions, wherein the overall crystal hit ratio (e.g., fraction of images with observable diffraction patterns) is a function of the microcrystal slurry concentration. We report crystal structures from lysozyme, thermolysin, and stachydrine demethylase (Stc2). Additional samples were screened to demonstrate that these methods can be applied to rare samples.
X-ray free-electron lasers (XFELs) provide very intense X-ray pulsn class="Chemical">es suitable for macromolecular crystallography. Each X-ray pulse typically lasts for tens of femtoseconds and the interval between pulses is many orders of magnitude longer. Here we describe two novel acoustic injection systems that use focused sound waves to eject picoliter to nanoliter crystal-containing droplets out of microplates and into the X-ray pulse from which diffraction data are collected. The on-demand droplet delivery is synchronized to the XFEL pulse scheme, resulting in X-ray pulses intersecting up to 88% of the droplets. We tested several types of samples in a range of crystallization conditions, wherein the overall crystal hit ratio (e.g., fraction of images with observable diffraction patterns) is a function of the microcrystal slurry concentration. We report crystal structures from lysozyme, thermolysin, and stachydrine demethylase (Stc2). Additional samples were screened to demonstrate that these methods can be applied to rare samples.
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