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Title: Lipidic cubic phase injector is a viable crystal delivery system for time-resolved serial crystallography

Journal Article · · Nature Communications
DOI:https://doi.org/10.1038/ncomms12314· OSTI ID:1313008
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  1. Paul Scherrer Inst. (PSI), Villigen (Switzerland)
  2. Arizona State Univ., Tempe, AZ (United States)
  3. Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany)
  4. RIKEN SPring-8 Center, Hyogo (Japan)
  5. SLAC National Accelerator Lab., Menlo Park, CA (United States)
  6. RIKEN SPring-8 Center, Hyogo (Japan); PRESTO, JST, Saitama (Japan)
  7. Univ. of Gothenburg, Gothenburg (Sweden)
  8. RIKEN/SPring-8 Center, Hyogo (Japan)
  9. RIKEN/SPring-8 Center, Hyogo (Japan); Kyoto Univ., Kyoto (Japan)
  10. Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany); Univ. of Hamburg, Hamburg (Germany)
  11. Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States)
  12. Paul Scherrer Inst. (PSI), Villigen (Switzerland); ETH Zurich, Zurich (Switzerland)

Serial femtosecond crystallography (SFX) using X-ray free-electron laser sources is an emerging method with considerable potential for time-resolved pump-probe experiments. Here we present a lipidic cubic phase SFX structure of the light-driven proton pump bacteriorhodopsin (bR) to 2.3 Å resolution and a method to investigate protein dynamics with modest sample requirement. Time-resolved SFX (TR-SFX) with a pump-probe delay of 1 ms yields difference Fourier maps compatible with the dark to M state transition of bR. Importantly, the method is very sample efficient and reduces sample consumption to about 1 mg per collected time point. Accumulation of M intermediate within the crystal lattice is confirmed by time-resolved visible absorption spectroscopy. This study provides an important step towards characterizing the complete photocycle dynamics of retinal proteins and demonstrates the feasibility of a sample efficient viscous medium jet for TR-SFX.

Research Organization:
SLAC National Accelerator Laboratory (SLAC), Menlo Park, CA (United States); Lawrence Livermore National Laboratory (LLNL), Livermore, CA (United States)
Sponsoring Organization:
USDOE Office of Science (SC), Basic Energy Sciences (BES); USDOE National Nuclear Security Administration (NNSA)
Grant/Contract Number:
AC02-76SF00515; AC52-07NA27344
OSTI ID:
1313008
Alternate ID(s):
OSTI ID: 1959522
Report Number(s):
LLNL-JRNL-844106; ncomms12314
Journal Information:
Nature Communications, Vol. 7; ISSN 2041-1723
Publisher:
Nature Publishing GroupCopyright Statement
Country of Publication:
United States
Language:
English
Citation Metrics:
Cited by: 69 works
Citation information provided by
Web of Science

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Hydroxyethyl cellulose matrix applied to serial crystallography journal April 2017
A fixed-target platform for serial femtosecond crystallography in a hydrated environment text January 2020
A three-dimensional movie of structural changes in bacteriorhodopsin journal December 2016
Structure-factor amplitude reconstruction from serial femtosecond crystallography of two-dimensional membrane-protein crystals text January 2019
Short-wavelength free-electron laser sources and science: a review journal October 2017
Perspective: Opportunities for ultrafast science at SwissFEL text January 2017
A temperature-controlled cold-gas humidifier and its application to protein crystals with the humid-air and glue-coating method text January 2019
Non-cryogenic structure of a chloride pump provides crucial clues to temperature-dependent channel transport efficiency journal November 2018
Microfluidics: From crystallization to serial time-resolved crystallography journal May 2017
Sample delivery for serial crystallography at free-electron lasers and synchrotrons journal January 2019
Capturing an initial intermediate during the P450nor enzymatic reaction using time-resolved XFEL crystallography and caged-substrate journal November 2017
Retinal isomerization in bacteriorhodopsin captured by a femtosecond x-ray laser journal June 2018
Perspective: Opportunities for ultrafast science at SwissFEL journal November 2017
On-chip crystallization for serial crystallography experiments and on-chip ligand-binding studies text January 2019
A temperature-controlled cold-gas humidifier and its application to protein crystals with the humid-air and glue-coating method journal June 2019
Pump-Probe Time-Resolved Serial Femtosecond Crystallography at SACLA: Current Status and Data Collection Strategies journal December 2019
On-chip crystallization for serial crystallography experiments and on-chip ligand-binding studies text January 2019
Perspective: Opportunities for ultrafast science at SwissFEL text January 2017
Flexible lipid nanomaterials studied by NMR spectroscopy journal January 2019
Structure-factor amplitude reconstruction from serial femtosecond crystallography of two-dimensional membrane-protein crystals journal January 2019
Time-resolved x-ray crystallography capture of a slow reaction tetrahydrofolate intermediate journal March 2019
The serial millisecond crystallography instrument at the Australian Synchrotron incorporating the “Lipidico” injector journal August 2019
Proton uptake mechanism in bacteriorhodopsin captured by serial synchrotron crystallography journal July 2019
Retinal isomerization in bacteriorhodopsin captured by a femtosecond x-ray laser text January 2018
Strategies for sample delivery for femtosecond crystallography text January 2019
Photoswitching mechanism of a fluorescent protein revealed by time-resolved crystallography and transient absorption spectroscopy journal February 2020
Short-wavelength free-electron laser sources and science: a review text January 2017
A guide to sample delivery systems for serial crystallography journal August 2019
SPIND : a reference-based auto-indexing algorithm for sparse serial crystallography data journal January 2019
Serial millisecond crystallography for routine room-temperature structure determination at synchrotrons journal September 2017
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Orientation of non-spherical protonated water clusters revealed by infrared absorption dichroism journal January 2018
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Figures / Tables (5)