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Demonstration of femtosecond X-ray pump X-ray probe diffraction on protein crystals

Journal Article · · Structural Dynamics
DOI:https://doi.org/10.1063/1.5050618· OSTI ID:2565518

The development of X-ray free-electron lasers (XFELs) has opened the possibility to investigate the ultrafast dynamics of biomacromolecules using X-ray diffraction. Whereas an increasing number of structures solved by means of serial femtosecond crystallography at XFELs is available, the effect of radiation damage on protein crystals during ultrafast exposures has remained an open question. We used a split-and-delay line based on diffractive X-ray optics at the Linac Coherent Light Source XFEL to investigate the time dependence of X-ray radiation damage to lysozyme crystals. For these tests, crystals were delivered to the X-ray beam using a fixed-target approach. The presented experiments provide probe signals at eight different delay times between 19 and 213 femtoseconds after a single pump event, thereby covering the time-scales relevant for femtosecond serial crystallography. Even though significant impact on the crystals was observed at long time scales after exposure with a single X-ray pulse, the collected diffraction data did not show significant signal reduction that could be assigned to beam damage on the crystals in the sampled time window and resolution range. This observation is in agreement with estimations of the applied radiation dose, which in our experiment was clearly below the values expected to cause damage on the femtosecond time scale. The experiments presented here demonstrate the feasibility of time-resolved pump-multiprobe X-ray diffraction experiments on protein crystals.

Research Organization:
Lawrence Livermore National Laboratory (LLNL), Livermore, CA (United States); SLAC National Accelerator Laboratory, Menlo Park, CA (United States). Linac Coherent Light Source (LCLS)
Sponsoring Organization:
European Community’s Seventh Framework Programme; Swiss Nanoscience Institute; USDOE; USDOE Office of Science (SC), Basic Energy Sciences (BES)
Grant/Contract Number:
AC02-76SF00515; AC52-07NA27344
OSTI ID:
2565518
Alternate ID(s):
OSTI ID: 1625000
OSTI ID: 1475093
Journal Information:
Structural Dynamics, Journal Name: Structural Dynamics Journal Issue: 5 Vol. 5; ISSN 2329-7778
Publisher:
American Institute of PhysicsCopyright Statement
Country of Publication:
United States
Language:
English

References (47)

Solvent content of protein crystals journal April 1968
Structure of the Angiotensin Receptor Revealed by Serial Femtosecond Crystallography journal May 2015
A Bright Future for Serial Femtosecond Crystallography with XFELs journal September 2017
Diffract-and-destroy: Can X-ray lasers “solve” the radiation damage problem? journal November 2008
X-ray Free Electron Laser Radiation Damage through the S-State Cycle of the Oxygen-Evolving Complex of Photosystem II journal September 2017
Potential for biomolecular imaging with femtosecond X-ray pulses journal August 2000
Europe’s X-ray laser fires up journal August 2017
Femtosecond X-ray protein nanocrystallography journal February 2011
Serial time-resolved crystallography of photosystem II using a femtosecond X-ray laser journal July 2014
Crystal structure of rhodopsin bound to arrestin by femtosecond X-ray laser journal July 2015
Structure of CPV17 polyhedrin determined by the improved analysis of serial femtosecond crystallographic data journal March 2015
Ultrafast myoglobin structural dynamics observed with an X-ray free-electron laser journal April 2015
Determination of damage-free crystal structure of an X-ray–sensitive protein using an XFEL journal May 2014
Grease matrix as a versatile carrier of proteins for serial crystallography journal November 2014
First lasing and operation of an ångstrom-wavelength free-electron laser journal August 2010
Self-terminating diffraction gates femtosecond X-ray nanocrystallography measurements journal December 2011
Nanofocusing of hard X-ray free electron laser pulses using diamond based Fresnel zone plates journal August 2011
Following the dynamics of matter with femtosecond precision using the X-ray streaking method journal January 2015
Electronic damage in S atoms in a native protein crystal induced by an intense X-ray free-electron laser pulse journal July 2015
A short history of structure based research on the photocycle of photoactive yellow protein journal May 2017
Observation of femtosecond X-ray interactions with matter using an X-ray–X-ray pump–probe scheme journal January 2016
Redox-coupled proton transfer mechanism in nitrite reductase revealed by femtosecond crystallography journal February 2016
XFEL structures of the influenza M2 proton channel: Room temperature water networks and insights into proton conduction journal August 2017
Diffraction before destruction journal July 2014
Radiation damage in protein serial femtosecond crystallography using an x-ray free-electron laser journal December 2011
Delayed Onset of Nonthermal Melting in Single-Crystal Silicon Pumped with Hard X Rays journal June 2018
X-ray powder diffraction analysis of silver behenate, a possible low-angle diffraction standard journal April 1993
Radiation damage in macromolecular crystallography: what is it and why should we care? journal March 2010
CrystalDirect: a new method for automated crystal harvesting based on laser-induced photoablation of thin films journal September 2012
Dose dependence of radiation damage for protein crystals studied at various X-ray energies journal December 2006
Direct protein crystallization on ultrathin membranes for diffraction measurements at X-ray free-electron lasers journal June 2017
Simulations of radiation damage as a function of the temporal pulse profile in femtosecond X-ray protein crystallography journal February 2015
Radiation damage to macromolecules: kill or cure? journal February 2015
X-ray detectors at the Linac Coherent Light Source journal April 2015
Performance of a hard X-ray split-and-delay optical system with a wavefront division journal January 2018
XFELs for structure and dynamics in biology journal May 2017
EIGER detector: application in macromolecular crystallography journal August 2016
Analysis of solvent content and oligomeric states in protein crystals-does symmetry matter? journal April 2008
The MEL-X project at the Lawrence Livermore National Laboratory: a mirror-based delay line for x-rays conference September 2015
A nanosecond time-resolved XFEL analysis of structural changes associated with CO release from cytochrome c oxidase journal July 2017
High-Resolution Protein Structure Determination by Serial Femtosecond Crystallography journal May 2012
Time-resolved serial crystallography captures high-resolution intermediates of photoactive yellow protein journal December 2014
A three-dimensional movie of structural changes in bacteriorhodopsin journal December 2016
Time-resolved protein nanocrystallography using an X-ray free-electron laser journal January 2012
Ultrafast self-gating Bragg diffraction of exploding nanocrystals in an X-ray laser journal January 2015
Single-shot analysis of hard x-ray laser radiation using a noninvasive grating spectrometer journal January 2012
Advances in X-ray free electron laser (XFEL) diffraction data processing applied to the crystal structure of the synaptotagmin-1 / SNARE complex journal October 2016