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Title: Fixed target matrix for femtosecond time-resolved and in situ serial micro-crystallography

Journal Article · · Structural Dynamics
DOI: https://doi.org/10.1063/1.4928706 · OSTI ID:1230061
 [1];  [2];  [2];  [2];  [1];  [1];  [3];  [4];  [5];  [6];  [7];  [8];  [3];  [4];  [1];  [9]
  1. Univ. of Toronto, Toronto, ON (Canada)
  2. Max Planck Institute for the Structure and Dynamics of Matter, Hamburg (Germany)
  3. Rice Univ., Houston, TX (United States)
  4. National Institutes of Health, Bethesda, MD (United States)
  5. SLAC National Accelerator Lab., Menlo Park, CA (United States)
  6. Diamond Light Source, Didcot (United Kingdom)
  7. Univ. of Toronto, Toronto, ON (Canada); Univ. of Toronto and Campbell Family Institute for Cancer Research, Univ. Health Network, Toronto, ON (Canada)
  8. Univ. of Hamburg, Hamburg (Germany)
  9. Univ. of Toronto, Toronto, ON (Canada); Max Planck Institute for the Structure and Dynamics of Matter, Hamburg (Germany); Univ. of Hamburg, Hamburg (Germany)

We present a crystallography chip enabling in situ room temperature crystallography at microfocus synchrotron beamlines and X-ray free-electron laser (X-FEL) sources. Compared to other in situ approaches, we observe extremely low background and high diffraction data quality. The chip design is robust and allows fast and efficient loading of thousands of small crystals. The ability to load a large number of protein crystals, at room temperature and with high efficiency, into prescribed positions enables high throughput automated serial crystallography with microfocus synchrotron beamlines. In addition, we demonstrate the application of this chip for femtosecond time-resolved serial crystallography at the Linac Coherent Light Source (LCLS, Menlo Park, California, USA). As a result, the chip concept enables multiple images to be acquired from each crystal, allowing differential detection of changes in diffraction intensities in order to obtain high signal-to-noise and fully exploit the time resolution capabilities of XFELs.

Research Organization:
SLAC National Accelerator Laboratory (SLAC), Menlo Park, CA (United States)
Sponsoring Organization:
USDOE Office of Science (SC)
Grant/Contract Number:
AC03-76SF00515
OSTI ID:
1230061
Journal Information:
Structural Dynamics, Journal Name: Structural Dynamics Journal Issue: 5 Vol. 2; ISSN SDTYAE; ISSN 2329-7778
Publisher:
American Crystallographic Association/AIPCopyright Statement
Country of Publication:
United States
Language:
English

References (51)

Crystal structure of myoglobin form a synthetic gene journal January 1990
Automated data collection for macromolecular crystallography journal September 2011
Energetics and Dynamics of Deterministic Protein Motion journal May 1994
Femtosecond electronic response of atoms to ultra-intense X-rays journal July 2010
Femtosecond X-ray protein nanocrystallography journal February 2011
Serial time-resolved crystallography of photosystem II using a femtosecond X-ray laser journal July 2014
Tracking the structural dynamics of proteins in solution using time-resolved wide-angle X-ray scattering journal September 2008
Structural biology: 'seeing' crystals the XFEL way journal August 2014
Achieving few-femtosecond time-sorting at hard X-ray free-electron lasers journal February 2013
A micro-patterned silicon chip as sample holder for macromolecular crystallography experiments with minimal background scattering journal May 2015
High-level expression of sperm whale myoglobin in Escherichia coli. journal December 1987
Scaling and assessment of data quality journal December 2005
Overview of the CCP 4 suite and current developments journal March 2011
Crystallography on a chip journal February 2012
Clustering procedures for the optimal selection of data sets from multiple crystals in macromolecular crystallography journal July 2013
The RATIO method for time-resolved Laue crystallography journal January 2009
High-Resolution Protein Structure Determination by Serial Femtosecond Crystallography journal May 2012
Molecular Imaging Using X-Ray Free-Electron Lasers journal April 2013
Mapping Atomic Motions with Ultrabright Electrons: The Chemists' Gedanken Experiment Enters the Lab Frame journal April 2014
Gas Dynamic Virtual Nozzle for Generation of Microscopic Droplet Streams text January 2008
Crystal structure of myoglobin form a synthetic gene journal January 1990
Automated data collection for macromolecular crystallography journal September 2011
Self-Localizing Stabilized Mega-Pixel Picoliter Arrays with Size-Exclusion Sorting Capabilities journal February 2011
Energetics and Dynamics of Deterministic Protein Motion journal May 1994
Potential for biomolecular imaging with femtosecond X-ray pulses journal August 2000
Femtosecond electronic response of atoms to ultra-intense X-rays journal July 2010
Femtosecond X-ray protein nanocrystallography journal February 2011
Serial time-resolved crystallography of photosystem II using a femtosecond X-ray laser journal July 2014
Tracking the structural dynamics of proteins in solution using time-resolved wide-angle X-ray scattering journal September 2008
Accurate macromolecular structures using minimal measurements from X-ray free-electron lasers journal March 2014
Structural biology: 'seeing' crystals the XFEL way journal August 2014
Achieving few-femtosecond time-sorting at hard X-ray free-electron lasers journal February 2013
A micro-patterned silicon chip as sample holder for macromolecular crystallography experiments with minimal background scattering journal May 2015
Watching a signaling protein function in real time via 100-ps time-resolved Laue crystallography journal November 2012
High-level expression of sperm whale myoglobin in Escherichia coli. journal December 1987
Gas dynamic virtual nozzle for generation of microscopic droplet streams journal September 2008
xia2 : an expert system for macromolecular crystallography data reduction journal December 2009
Scaling and assessment of data quality journal December 2005
XDS journal January 2010
Overview of the CCP 4 suite and current developments journal March 2011
In-plate protein crystallization, in situ ligand soaking and X-ray diffraction journal August 2011
Crystallography on a chip journal February 2012
Clustering procedures for the optimal selection of data sets from multiple crystals in macromolecular crystallography journal July 2013
The RATIO method for time-resolved Laue crystallography journal January 2009
Breaking the indexing ambiguity in serial crystallography journal December 2013
Watching a Protein as it Functions with 150-ps Time-Resolved X-ray Crystallography journal June 2003
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
Molecular Imaging Using X-Ray Free-Electron Lasers journal April 2013
Mapping Atomic Motions with Ultrabright Electrons: The Chemists' Gedanken Experiment Enters the Lab Frame journal April 2014
Overview of the CCP4 suite and current developments. text January 2011

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Short-wavelength free-electron laser sources and science: a review text January 2017
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SwissFEL: The Swiss X-ray Free Electron Laser journal July 2017
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