skip to main content
DOE PAGES title logo U.S. Department of Energy
Office of Scientific and Technical Information

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

Abstract

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.

Authors:
 [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)
Publication Date:
Research Org.:
SLAC National Accelerator Lab., Menlo Park, CA (United States)
Sponsoring Org.:
USDOE Office of Science (SC)
OSTI Identifier:
1230061
Grant/Contract Number:  
AC03-76SF00515
Resource Type:
Accepted Manuscript
Journal Name:
Structural Dynamics
Additional Journal Information:
Journal Volume: 2; Journal Issue: 5; Journal ID: ISSN 2329-7778
Publisher:
American Crystallographic Association/AIP
Country of Publication:
United States
Language:
English
Subject:
75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND SUPERFLUIDITY; X-ray diffraction; crystal structure; proteins; crystallization; time dependent material structure

Citation Formats

Mueller, C., Marx, A., Epp, S. W., Zhong, Y., Kuo, A., Balo, A. R., Soman, J., Schotte, F., Lemke, H. T., Owen, R. L., Pai, E. F., Pearson, A. R., Olson, J. S., Anfinrud, P. A., Ernst, O. P., and Miller, R. J. Dwayne. Fixed target matrix for femtosecond time-resolved and in situ serial micro-crystallography. United States: N. p., 2015. Web. doi:10.1063/1.4928706.
Mueller, C., Marx, A., Epp, S. W., Zhong, Y., Kuo, A., Balo, A. R., Soman, J., Schotte, F., Lemke, H. T., Owen, R. L., Pai, E. F., Pearson, A. R., Olson, J. S., Anfinrud, P. A., Ernst, O. P., & Miller, R. J. Dwayne. Fixed target matrix for femtosecond time-resolved and in situ serial micro-crystallography. United States. doi:https://doi.org/10.1063/1.4928706
Mueller, C., Marx, A., Epp, S. W., Zhong, Y., Kuo, A., Balo, A. R., Soman, J., Schotte, F., Lemke, H. T., Owen, R. L., Pai, E. F., Pearson, A. R., Olson, J. S., Anfinrud, P. A., Ernst, O. P., and Miller, R. J. Dwayne. Tue . "Fixed target matrix for femtosecond time-resolved and in situ serial micro-crystallography". United States. doi:https://doi.org/10.1063/1.4928706. https://www.osti.gov/servlets/purl/1230061.
@article{osti_1230061,
title = {Fixed target matrix for femtosecond time-resolved and in situ serial micro-crystallography},
author = {Mueller, C. and Marx, A. and Epp, S. W. and Zhong, Y. and Kuo, A. and Balo, A. R. and Soman, J. and Schotte, F. and Lemke, H. T. and Owen, R. L. and Pai, E. F. and Pearson, A. R. and Olson, J. S. and Anfinrud, P. A. and Ernst, O. P. and Miller, R. J. Dwayne},
abstractNote = {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.},
doi = {10.1063/1.4928706},
journal = {Structural Dynamics},
number = 5,
volume = 2,
place = {United States},
year = {2015},
month = {8}
}

Journal Article:
Free Publicly Available Full Text
Publisher's Version of Record

Citation Metrics:
Cited by: 23 works
Citation information provided by
Web of Science

Save / Share:

Works referenced in this record:

Energetics and Dynamics of Deterministic Protein Motion
journal, May 1994

  • Miller, R. J. Dwayne
  • Accounts of Chemical Research, Vol. 27, Issue 5
  • DOI: 10.1021/ar00041a005

Mapping Atomic Motions with Ultrabright Electrons: The Chemists' Gedanken Experiment Enters the Lab Frame
journal, April 2014


Potential for biomolecular imaging with femtosecond X-ray pulses
journal, August 2000

  • Neutze, Richard; Wouts, Remco; van der Spoel, David
  • Nature, Vol. 406, Issue 6797
  • DOI: 10.1038/35021099

Molecular Imaging Using X-Ray Free-Electron Lasers
journal, April 2013


Femtosecond electronic response of atoms to ultra-intense X-rays
journal, July 2010


Femtosecond X-ray protein nanocrystallography
journal, February 2011

  • Chapman, Henry N.; Fromme, Petra; Barty, Anton
  • Nature, Vol. 470, Issue 7332, p. 73-77
  • DOI: 10.1038/nature09750

Structural biology: 'seeing' crystals the XFEL way
journal, August 2014


Tracking the structural dynamics of proteins in solution using time-resolved wide-angle X-ray scattering
journal, September 2008

  • Cammarata, Marco; Levantino, Matteo; Schotte, Friedrich
  • Nature Methods, Vol. 5, Issue 10
  • DOI: 10.1038/nmeth.1255

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


Watching a signaling protein function in real time via 100-ps time-resolved Laue crystallography
journal, November 2012

  • Schotte, F.; Cho, H. S.; Kaila, V. R. I.
  • Proceedings of the National Academy of Sciences, Vol. 109, Issue 47
  • DOI: 10.1073/pnas.1210938109

Crystallography on a chip
journal, February 2012

  • Zarrine-Afsar, Arash; Barends, Thomas R. M.; Müller, Christina
  • Acta Crystallographica Section D Biological Crystallography, Vol. 68, Issue 3
  • DOI: 10.1107/S0907444911055296

In-plate protein crystallization, in situ ligand soaking and X-ray diffraction
journal, August 2011

  • le Maire, Albane; Gelin, Muriel; Pochet, Sylvie
  • Acta Crystallographica Section D Biological Crystallography, Vol. 67, Issue 9
  • DOI: 10.1107/S0907444911023249

Automated data collection for macromolecular crystallography
journal, September 2011


Clustering procedures for the optimal selection of data sets from multiple crystals in macromolecular crystallography
journal, July 2013

  • Foadi, James; Aller, Pierre; Alguel, Yilmaz
  • Acta Crystallographica Section D Biological Crystallography, Vol. 69, Issue 8
  • DOI: 10.1107/S0907444913012274

The RATIO method for time-resolved Laue crystallography
journal, January 2009

  • Coppens, Philip; Pitak, Mateusz; Gembicky, Milan
  • Journal of Synchrotron Radiation, Vol. 16, Issue 2
  • DOI: 10.1107/S0909049508040892

Breaking the indexing ambiguity in serial crystallography
journal, December 2013

  • Brehm, Wolfgang; Diederichs, Kay
  • Acta Crystallographica Section D Biological Crystallography, Vol. 70, Issue 1
  • DOI: 10.1107/S1399004713025431

Gas dynamic virtual nozzle for generation of microscopic droplet streams
journal, September 2008

  • DePonte, D. P.; Weierstall, U.; Schmidt, K.
  • Journal of Physics D: Applied Physics, Vol. 41, Issue 19, Article No. 195505
  • DOI: 10.1088/0022-3727/41/19/195505

Serial time-resolved crystallography of photosystem II using a femtosecond X-ray laser
journal, July 2014

  • Kupitz, Christopher; Basu, Shibom; Grotjohann, Ingo
  • Nature, Vol. 513, Issue 7517
  • DOI: 10.1038/nature13453

Accurate macromolecular structures using minimal measurements from X-ray free-electron lasers
journal, March 2014

  • Hattne, Johan; Echols, Nathaniel; Tran, Rosalie
  • Nature Methods, Vol. 11, Issue 5
  • DOI: 10.1038/nmeth.2887

High-level expression of sperm whale myoglobin in Escherichia coli.
journal, December 1987

  • Springer, B. A.; Sligar, S. G.
  • Proceedings of the National Academy of Sciences, Vol. 84, Issue 24
  • DOI: 10.1073/pnas.84.24.8961

Crystal structure of myoglobin form a synthetic gene
journal, January 1990

  • Phillips, George N.; Arduini, Robert M.; Springer, Barry A.
  • Proteins: Structure, Function, and Genetics, Vol. 7, Issue 4
  • DOI: 10.1002/prot.340070407

Self-Localizing Stabilized Mega-Pixel Picoliter Arrays with Size-Exclusion Sorting Capabilities
journal, February 2011

  • Zarrine-Afsar, Arash; Müller, Christina; Talbot, Francis O.
  • Analytical Chemistry, Vol. 83, Issue 3
  • DOI: 10.1021/ac1021024

Achieving few-femtosecond time-sorting at hard X-ray free-electron lasers
journal, February 2013


xia2 : an expert system for macromolecular crystallography data reduction
journal, December 2009


Overview of the CCP 4 suite and current developments
journal, March 2011

  • Winn, Martyn D.; Ballard, Charles C.; Cowtan, Kevin D.
  • Acta Crystallographica Section D Biological Crystallography, Vol. 67, Issue 4
  • DOI: 10.1107/S0907444910045749

XDS
journal, January 2010

  • Kabsch, Wolfgang
  • Acta Crystallographica Section D Biological Crystallography, Vol. 66, Issue 2
  • DOI: 10.1107/S0907444909047337

Scaling and assessment of data quality
journal, December 2005

  • Evans, Philip
  • Acta Crystallographica Section D Biological Crystallography, Vol. 62, Issue 1, p. 72-82
  • DOI: 10.1107/S0907444905036693

A micro-patterned silicon chip as sample holder for macromolecular crystallography experiments with minimal background scattering
journal, May 2015

  • Roedig, P.; Vartiainen, I.; Duman, R.
  • Scientific Reports, Vol. 5, Issue 1
  • DOI: 10.1038/srep10451

    Works referencing / citing this record:

    Room-temperature macromolecular crystallography using a micro-patterned silicon chip with minimal background scattering
    journal, May 2016

    • Roedig, Philip; Duman, Ramona; Sanchez-Weatherby, Juan
    • Journal of Applied Crystallography, Vol. 49, Issue 3
    • DOI: 10.1107/s1600576716006348

    Dose-resolved serial synchrotron and XFEL structures of radiation-sensitive metalloproteins
    journal, May 2019


    Nylon mesh-based sample holder for fixed-target serial femtosecond crystallography
    journal, May 2019


    Fixed-target serial oscillation crystallography at room temperature
    journal, February 2019


    Nylon mesh-based sample holder for fixed-target serial femtosecond crystallography
    journal, May 2019


    Room-temperature macromolecular crystallography using a micro-patterned silicon chip with minimal background scattering
    journal, May 2016

    • Roedig, Philip; Duman, Ramona; Sanchez-Weatherby, Juan
    • Journal of Applied Crystallography, Vol. 49, Issue 3
    • DOI: 10.1107/s1600576716006348

    Fixed-target serial oscillation crystallography at room temperature
    journal, February 2019


    Dose-resolved serial synchrotron and XFEL structures of radiation-sensitive metalloproteins
    journal, May 2019


    Room-Temperature Macromolecular Crystallography Using a Micro-Patterned Silicon Chip with Minimal Background Scattering
    text, January 2016

    • Roedig, Philip; Duman, Ramona; Sanchez-Weatherby, Juan
    • Deutsches Elektronen-Synchrotron, DESY, Hamburg
    • DOI: 10.3204/pubdb-2016-02690

    DIY XES-development of an inexpensive, versatile, and easy to fabricate XES analyzer and sample delivery system
    journal, February 2019

    • Jensen, Scott C.; Sullivan, Brendan; Hartzler, Daniel A.
    • X-Ray Spectrometry, Vol. 48, Issue 5
    • DOI: 10.1002/xrs.3005

    High-speed fixed-target serial virus crystallography
    journal, June 2017

    • Roedig, Philip; Ginn, Helen M.; Pakendorf, Tim
    • Nature Methods, Vol. 14, Issue 8
    • DOI: 10.1038/nmeth.4335

    High-throughput in situ X-ray screening of and data collection from protein crystals at room temperature and under cryogenic conditions
    journal, January 2018

    • Broecker, Jana; Morizumi, Takefumi; Ou, Wei-Lin
    • Nature Protocols, Vol. 13, Issue 2
    • DOI: 10.1038/nprot.2017.135

    Serial protein crystallography in an electron microscope
    journal, February 2020


    Watching proteins function with time-resolved x-ray crystallography
    journal, August 2017

    • Šrajer, Vukica; Schmidt, Marius
    • Journal of Physics D: Applied Physics, Vol. 50, Issue 37
    • DOI: 10.1088/1361-6463/aa7d32

    Protein crystals IR laser ablated from aqueous solution at high speed retain their diffractive properties: applications in high-speed serial crystallography
    journal, November 2017

    • Schulz, Eike C.; Kaub, Johannes; Busse, Frederik
    • Journal of Applied Crystallography, Vol. 50, Issue 6
    • DOI: 10.1107/s1600576717014479

    3D printed droplet generation devices for serial femtosecond crystallography enabled by surface coating
    journal, August 2019

    • Echelmeier, Austin; Kim, Daihyun; Cruz Villarreal, Jorvani
    • Journal of Applied Crystallography, Vol. 52, Issue 5
    • DOI: 10.1107/s1600576719010343

    A modular and compact portable mini-endstation for high-precision, high-speed fixed target serial crystallography at FEL and synchrotron sources
    journal, October 2015

    • Sherrell, Darren A.; Foster, Andrew J.; Hudson, Lee
    • Journal of Synchrotron Radiation, Vol. 22, Issue 6
    • DOI: 10.1107/s1600577515016938

    A microfluidic flow-focusing device for low sample consumption serial synchrotron crystallography experiments in liquid flow
    journal, February 2019

    • Monteiro, Diana C. F.; Vakili, Mohammad; Harich, Jessica
    • Journal of Synchrotron Radiation, Vol. 26, Issue 2
    • DOI: 10.1107/s1600577519000304

    A multicrystal diffraction data-collection approach for studying structural dynamics with millisecond temporal resolution
    journal, October 2016


    Lifetimes and spatio-temporal response of protein crystals in intense X-ray microbeams
    journal, October 2017


    Sample manipulation and data assembly for robust microcrystal synchrotron crystallography
    journal, April 2018


    Fixed target combined with spectral mapping: approaching 100% hit rates for serial crystallography
    journal, July 2016

    • Oghbaey, Saeed; Sarracini, Antoine; Ginn, Helen M.
    • Acta Crystallographica Section D Structural Biology, Vol. 72, Issue 8, p. 944-955
    • DOI: 10.1107/s2059798316010834

    Low-dose fixed-target serial synchrotron crystallography
    journal, March 2017

    • Owen, Robin L.; Axford, Danny; Sherrell, Darren A.
    • Acta Crystallographica Section D Structural Biology, Vol. 73, Issue 4, p. 373-378
    • DOI: 10.1107/s2059798317002996

    Crystallography on a chip – without the chip: sheet-on-sheet sandwich
    journal, October 2018

    • Doak, R. Bruce; Nass Kovacs, Gabriela; Gorel, Alexander
    • Acta Crystallographica Section D Structural Biology, Vol. 74, Issue 10
    • DOI: 10.1107/s2059798318011634

    Strategies for sample delivery for femtosecond crystallography
    journal, February 2019

    • Martiel, Isabelle; Müller-Werkmeister, Henrike M.; Cohen, Aina E.
    • Acta Crystallographica Section D Structural Biology, Vol. 75, Issue 2
    • DOI: 10.1107/s2059798318017953

    SwissFEL: The Swiss X-ray Free Electron Laser
    journal, July 2017

    • Milne, Christopher; Schietinger, Thomas; Aiba, Masamitsu
    • Applied Sciences, Vol. 7, Issue 7
    • DOI: 10.3390/app7070720