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

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. Furthermore, 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.
Authors:
ORCiD logo [1] ;  [1] ;  [2] ;  [3] ;  [4] ; ORCiD logo [1] ;  [5] ;  [6] ;  [1] ;  [2] ;  [2] ;  [3] ;  [2] ;  [7] ;  [7] ;  [7] ;  [3] ;  [1] ; ORCiD logo [1] ;  [5] more »;  [2] ;  [1] ;  [5] ;  [5] ; ORCiD logo [5] ;  [7] ;  [8] ;  [9] ; ORCiD logo [10] ;  [2] ; ORCiD logo [11] ;  [1] ;  [5] ;  [3] ;  [3] ;  [2] ;  [2] ;  [7] ;  [12] ;  [1] « less
  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)
Publication Date:
Grant/Contract Number:
AC02-76SF00515
Type:
Accepted Manuscript
Journal Name:
Nature Communications
Additional Journal Information:
Journal Volume: 7; Journal ID: ISSN 2041-1723
Publisher:
Nature Publishing Group
Research Org:
SLAC National Accelerator Lab., Menlo Park, CA (United States)
Sponsoring Org:
USDOE
Country of Publication:
United States
Language:
English
Subject:
59 BASIC BIOLOGICAL SCIENCES
OSTI Identifier:
1313008

Nogly, Przemyslaw, Panneels, Valerie, Nelson, Garrett, Gati, Cornelius, Kimura, Tetsunari, Milne, Christopher, Milathianaki, Despina, Kubo, Minoru, Wu, Wenting, Conrad, Chelsie, Coe, Jesse, Bean, Richard, Zhao, Yun, Bath, Petra, Dods, Robert, Harimoorthy, Rajiv, Beyerlein, Kenneth R., Rheinberger, Jan, James, Daniel, DePonte, Daniel, Li, Chufeng, Sala, Leonardo, Williams, Garth J., Hunter, Mark S., Koglin, Jason E., Berntsen, Peter, Nango, Eriko, Iwata, So, Chapman, Henry N., Fromme, Petra, Frank, Matthias, Abela, Rafael, Boutet, Sebastien, Barty, Anton, White, Thomas A., Weierstall, Uwe, Spence, John, Neutze, Richard, Schertler, Gebhard, and Standfuss, Jorg. Lipidic cubic phase injector is a viable crystal delivery system for time-resolved serial crystallography. United States: N. p., Web. doi:10.1038/ncomms12314.
Nogly, Przemyslaw, Panneels, Valerie, Nelson, Garrett, Gati, Cornelius, Kimura, Tetsunari, Milne, Christopher, Milathianaki, Despina, Kubo, Minoru, Wu, Wenting, Conrad, Chelsie, Coe, Jesse, Bean, Richard, Zhao, Yun, Bath, Petra, Dods, Robert, Harimoorthy, Rajiv, Beyerlein, Kenneth R., Rheinberger, Jan, James, Daniel, DePonte, Daniel, Li, Chufeng, Sala, Leonardo, Williams, Garth J., Hunter, Mark S., Koglin, Jason E., Berntsen, Peter, Nango, Eriko, Iwata, So, Chapman, Henry N., Fromme, Petra, Frank, Matthias, Abela, Rafael, Boutet, Sebastien, Barty, Anton, White, Thomas A., Weierstall, Uwe, Spence, John, Neutze, Richard, Schertler, Gebhard, & Standfuss, Jorg. Lipidic cubic phase injector is a viable crystal delivery system for time-resolved serial crystallography. United States. doi:10.1038/ncomms12314.
Nogly, Przemyslaw, Panneels, Valerie, Nelson, Garrett, Gati, Cornelius, Kimura, Tetsunari, Milne, Christopher, Milathianaki, Despina, Kubo, Minoru, Wu, Wenting, Conrad, Chelsie, Coe, Jesse, Bean, Richard, Zhao, Yun, Bath, Petra, Dods, Robert, Harimoorthy, Rajiv, Beyerlein, Kenneth R., Rheinberger, Jan, James, Daniel, DePonte, Daniel, Li, Chufeng, Sala, Leonardo, Williams, Garth J., Hunter, Mark S., Koglin, Jason E., Berntsen, Peter, Nango, Eriko, Iwata, So, Chapman, Henry N., Fromme, Petra, Frank, Matthias, Abela, Rafael, Boutet, Sebastien, Barty, Anton, White, Thomas A., Weierstall, Uwe, Spence, John, Neutze, Richard, Schertler, Gebhard, and Standfuss, Jorg. 2016. "Lipidic cubic phase injector is a viable crystal delivery system for time-resolved serial crystallography". United States. doi:10.1038/ncomms12314. https://www.osti.gov/servlets/purl/1313008.
@article{osti_1313008,
title = {Lipidic cubic phase injector is a viable crystal delivery system for time-resolved serial crystallography},
author = {Nogly, Przemyslaw and Panneels, Valerie and Nelson, Garrett and Gati, Cornelius and Kimura, Tetsunari and Milne, Christopher and Milathianaki, Despina and Kubo, Minoru and Wu, Wenting and Conrad, Chelsie and Coe, Jesse and Bean, Richard and Zhao, Yun and Bath, Petra and Dods, Robert and Harimoorthy, Rajiv and Beyerlein, Kenneth R. and Rheinberger, Jan and James, Daniel and DePonte, Daniel and Li, Chufeng and Sala, Leonardo and Williams, Garth J. and Hunter, Mark S. and Koglin, Jason E. and Berntsen, Peter and Nango, Eriko and Iwata, So and Chapman, Henry N. and Fromme, Petra and Frank, Matthias and Abela, Rafael and Boutet, Sebastien and Barty, Anton and White, Thomas A. and Weierstall, Uwe and Spence, John and Neutze, Richard and Schertler, Gebhard and Standfuss, Jorg},
abstractNote = {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. Furthermore, 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.},
doi = {10.1038/ncomms12314},
journal = {Nature Communications},
number = ,
volume = 7,
place = {United States},
year = {2016},
month = {8}
}

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