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Title: Pink-beam serial crystallography

Journal Article · · Nature Communications
ORCiD logo [1]; ORCiD logo [2];  [3];  [4];  [5];  [5];  [5];  [6];  [5];  [7];  [8];  [9];  [10];  [10]; ORCiD logo [6];  [6];  [8];  [5]; ORCiD logo [10]; ORCiD logo [11]
  1. DESY, Hamburg (Germany). Center for Free Electron Laser Science and Photon Science
  2. DESY, Hamburg (Germany). Center for Free Electron Laser Science; University of Hamburg (Germany). Dept. of Physics
  3. Univ. of Chicago, IL (United States). Center for Advanced Radiation Sources
  4. Center for Advanced Radiation Sources
  5. DESY, Hamburg (Germany). Center for Free Electron Laser Science
  6. Institut für Biophysikalische Chemie, Hannover (Germany). Medizinische Hochschule Hannover (MHH)
  7. University of Hamburg (Germany). Dept. of Physics
  8. Deutsches Elektronen Synchrotron (DESY), Hamburg (Germany). Photon Science
  9. National Science Foundation BioXFEL Science and Technology Center, Buffalo, NY (United States)
  10. Argonne National Lab. (ANL), Argonne, IL (United States). Advanced Photon Source (APS)
  11. DESY, Hamburg (Germany). Center for Free Electron Laser Science; University of Hamburg (Germany). Dept. of Physics; Centre for Ultrafast Imaging, Hamburg (Germany)

Serial X-ray crystallography allows macromolecular structure determination at both X-ray free electron lasers (XFELs) and, more recently, synchrotron sources. The time resolution for serial synchrotron crystallography experiments has been limited to millisecond timescales with monochromatic beams. The polychromatic, “pink”, beam provides a more than two orders of magnitude increased photon flux and hence allows accessing much shorter timescales in diffraction experiments at synchrotron sources. Here we report the structure determination of two different protein samples by merging pink-beam diffraction patterns from many crystals, each collected with a single 100 ps X-ray pulse exposure per crystal using a setup optimized for very low scattering background. In contrast to experiments with monochromatic radiation, data from only 50 crystals were required to obtain complete datasets. The high quality of the diffraction data highlights the potential of this method for studying irreversible reactions at sub-microsecond timescales using high-brightness X-ray facilities.

Research Organization:
Argonne National Laboratory (ANL), Argonne, IL (United States)
Sponsoring Organization:
USDOE Office of Science (SC), Basic Energy Sciences (BES) (SC-22). Scientific User Facilities Division; European Union - Horizon 2020 Research and Innovation Programme; Helmholtz Association of German Research Centres - Virtual Institute; National Institutes of Health (NIH) - National Institute of General Medical Sciences
Grant/Contract Number:
AC02-06CH11357
OSTI ID:
1422407
Journal Information:
Nature Communications, Journal Name: Nature Communications Journal Issue: 1 Vol. 8; ISSN 2041-1723
Publisher:
Nature Publishing GroupCopyright Statement
Country of Publication:
United States
Language:
English

References (65)

X-ray crystallographic structure of the light-harvesting biliprotein C-phycocyanin from the thermophilic cyanobacterium Mastigocladus laminosus and its resemblance to globin structures journal July 1985
The 1.45Å three-dimensional structure of C-phycocyanin from the thermophilic cyanobacterium Synechococcus elongatus journal February 2003
Kinetic Modeling of the X-ray-Induced Damage to a Metalloprotein journal July 2013
Millisecond Laue structures of an enzyme–product complex using photocaged substrate analogs journal October 1998
Time-resolved X-ray crystallographic study of the conformational change in Ha-Ras p21 protein on GTP hydrolysis journal May 1990
Femtosecond X-ray protein nanocrystallography journal February 2011
De novo phasing with X-ray laser reveals mosquito larvicide BinAB structure journal September 2016
Structures of riboswitch RNA reaction states by mix-and-inject XFEL serial crystallography journal November 2016
Imaging live cell in micro-liquid enclosure by X-ray laser diffraction journal January 2014
High-speed fixed-target serial virus crystallography journal June 2017
PARP1 exhibits enhanced association and catalytic efficiency with γH2A.X-nucleosome journal December 2019
A micro-patterned silicon chip as sample holder for macromolecular crystallography experiments with minimal background scattering journal May 2015
Structural enzymology using X-ray free electron lasers journal December 2016
Protein kinetics: Structures of intermediates and reaction mechanism from time-resolved x-ray data journal March 2004
From The Cover: Visualizing reaction pathways in photoactive yellow protein from nanoseconds to seconds journal May 2005
Ligand migration pathway and protein dynamics in myoglobin: A time-resolved crystallographic study on L29W MbCO journal August 2005
Allosteric action in real time: Time-resolved crystallographic studies of a cooperative dimeric hemoglobin journal May 2006
Experimental determination of the radiation dose limit for cryocooled protein crystals journal March 2006
Origin and temperature dependence of radiation damage in biological samples at cryogenic temperatures journal December 2009
Accessing protein conformational ensembles using room-temperature X-ray crystallography journal September 2011
Protein crystal structure obtained at 2.9 A resolution from injecting bacterial cells into an X-ray free-electron laser beam journal August 2014
Atomic structure of granulin determined from native nanocrystalline granulovirus using an X-ray free-electron laser journal February 2017
AGIPD, a high dynamic range fast detector for the European XFEL journal January 2015
Characterization results of the JUNGFRAU full scale readout ASIC journal February 2016
The Protein Data Bank journal January 2000
Using a non-monochromatic microbeam for serial snapshot crystallography journal April 2013
The recording and analysis of synchrotron X-radiation Laue diffraction photographs journal October 1989
Laue film integration and deconvolution of spatially overlapping reflections journal June 1990
The mosaic spread of very small crystals deduced from Laue diffraction patterns journal January 1987
Synchrotron X-ray data collection and restrained least-squares refinement of the crystal structure of proteinase K at 1.5 Å resolution journal April 1988
Towards automated Laue data processing: application to the choice of optimal X-ray spectrum journal August 2000
electronic Ligand Builder and Optimization Workbench ( eLBOW ): a tool for ligand coordinate and restraint generation journal September 2009
Features and development of Coot journal March 2010
Overview of the CCP 4 suite and current developments journal March 2011
Towards automated crystallographic structure refinement with phenix.refine journal March 2012
Outrunning free radicals in room-temperature macromolecular crystallography journal June 2012
Protein energy landscapes determined by five-dimensional crystallography journal November 2013
BioCARS: a synchrotron resource for time-resolved X-ray science journal May 2011
Laue Crystallography for Studying Rapid Reactions journal October 1994
Laue crystallography: coming of age journal July 1999
Room-temperature serial crystallography at synchrotron X-ray sources using slowly flowing free-standing high-viscosity microstreams journal January 2015
Capture and X-ray diffraction studies of protein microcrystals in a microfluidic trap array journal March 2015
Raster-scanning serial protein crystallography using micro- and nano-focused synchrotron beams journal April 2015
In meso in situ serial X-ray crystallography of soluble and membrane proteins journal May 2015
Room-temperature macromolecular crystallography using a micro-patterned silicon chip with minimal background scattering journal May 2016
Room-temperature macromolecular serial crystallography using synchrotron radiation journal May 2014
Lipidic cubic phase serial millisecond crystallography using synchrotron radiation journal March 2015
Serial femtosecond crystallography of soluble proteins in lipidic cubic phase journal August 2015
Serial millisecond crystallography of membrane and soluble protein microcrystals using synchrotron radiation journal May 2017
In-vacuum long-wavelength macromolecular crystallography journal March 2016
Low-dose fixed-target serial synchrotron crystallography journal March 2017
Using a non-monochromatic microbeam for serial snapshot crystallography journal August 2013
Structures of riboswitch RNA reaction states by mix-and-inject XFEL serial crystallography journal May 2017
The Protein Data Bank journal May 2002
Watching a Protein as it Functions with 150-ps Time-Resolved X-ray Crystallography journal June 2003
Light-Induced Structural Changes in a Photosynthetic Reaction Center Caught by Laue Diffraction journal April 2010
Photolysis of the Carbon Monoxide Complex of Myoglobin: Nanosecond Time-Resolved Crystallography journal December 1996
Biostructural Science Inspired by Next-Generation X-Ray Sources journal June 2015
Mix and Inject: Reaction Initiation by Diffusion for Time-Resolved Macromolecular Crystallography journal January 2013
Overview of the CCP4 suite and current developments. text January 2011
Serial femtosecond crystallography of soluble proteins in lipidic cubic phase text January 2015
Room-Temperature Macromolecular Crystallography Using a Micro-Patterned Silicon Chip with Minimal Background Scattering text January 2016
Structures of riboswitch RNA reaction states by mix-and-inject XFEL serial crystallography text January 2016
Structural enzymology using X-ray free electron lasers text January 2017
Lipidic cubic phase serial millisecond crystallography using synchrotron radiation text January 2015

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Sample delivery for serial crystallography at free-electron lasers and synchrotrons journal January 2019
Journey to the center of the protein: allostery from multitemperature multiconformer X-ray crystallography journal January 2019
Strategies for sample delivery for femtosecond crystallography journal February 2019
Strategies for sample delivery for femtosecond crystallography text January 2019
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Dose efficient Compton X-ray microscopy journal January 2018
Dose efficient Compton X-ray microscopy text January 2018
A detector for the sources text January 2018
On-chip crystallization for serial crystallography experiments and on-chip ligand-binding studies text January 2019