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

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

doi:10.1063/1.4928706

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:

Mueller, C. ^[1]; Marx, A. ^[2]; Epp, S. W. ^[2]; Zhong, Y. ^[2]; Kuo, A. ^[1]; Balo, A. R. ^[1]; Soman, J. ^[3]; Schotte, F. ^[4]; Lemke, H. T. ^[5]; Owen, R. L. ^[6]; Pai, E. F. ^[7]; Pearson, A. R. ^[8]; Olson, J. S. ^[3]; Anfinrud, P. A. ^[4]; Ernst, O. P. ^[1]; Miller, R. J. Dwayne ^[9]

Univ. of Toronto, Toronto, ON (Canada)
Max Planck Institute for the Structure and Dynamics of Matter, Hamburg (Germany)
Rice Univ., Houston, TX (United States)
National Institutes of Health, Bethesda, MD (United States)
SLAC National Accelerator Lab., Menlo Park, CA (United States)
Diamond Light Source, Didcot (United Kingdom)
Univ. of Toronto, Toronto, ON (Canada); Univ. of Toronto and Campbell Family Institute for Cancer Research, Univ. Health Network, Toronto, ON (Canada)
Univ. of Hamburg, Hamburg (Germany)
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:: Tue Aug 18 00:00:00 EDT 2015

Research Org.:: SLAC National Accelerator Laboratory (SLAC), 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.

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                    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.  https://doi.org/10.1063/1.4928706

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                    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.  https://doi.org/10.1063/1.4928706.  https://www.osti.gov/servlets/purl/1230061.

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@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         = {Tue Aug 18 00:00:00 EDT 2015},

  month        = {Tue Aug 18 00:00:00 EDT 2015}

}

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DOI: 10.1107/s2059798318010240/ba5292sup1.pdf

Fixed-target serial oscillation crystallography at room temperature
text, January 2019

Wierman, Jennifer L.; Paré-Labrosse, Olivier; Sarracini, Antoine
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DOI: 10.1107/s2052252519001453/mf5030sup1.pdf

Dose-resolved serial synchrotron and XFEL structures of radiation-sensitive metalloproteins
text, January 2019

Ebrahim, Ali; Moreno-Chicano, Tadeo; Appleby, Martin V.
International Union of Crystallography (IUCr)
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Serial protein crystallography in an electron microscope
text, January 2020

Bücker, Robert; Hogan-Lamarre, Pascal; Mehrabi, Pedram
Nature Publishing Group UK
DOI: 10.15480/882.2722

Short-wavelength free-electron laser sources and science: a review
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Seddon, E. A.; Clarke, J. A.; Dunning, D. J.
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DOI: 10.1088/1361-6633/aa7cca

A Versatile System for High-Throughput In Situ X-ray Screening and Data Collection of Soluble and Membrane-Protein Crystals
journal, October 2016

Broecker, Jana; Klingel, Viviane; Ou, Wei-Lin
Crystal Growth & Design, Vol. 16, Issue 11
DOI: 10.1021/acs.cgd.6b00950

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

Lee, Donghyeon; Baek, Sangwon; Park, Jaehyun
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DOI: 10.1038/s41598-019-43485-z

Time zero determination for FEL pump-probe studies based on ultrafast melting of bismuth
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Epp, S. W.; Hada, M.; Zhong, Y.
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The crystal structure of dGTPase reveals the molecular basis of dGTP selectivity
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SwissFEL: The Swiss X-ray Free Electron Laser
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DOI: 10.3390/app7070720

Sample Delivery Media for Serial Crystallography
journal, March 2019

Nam, Ki
International Journal of Molecular Sciences, Vol. 20, Issue 5
DOI: 10.3390/ijms20051094

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

Abstract

Citation Formats

Energetics and Dynamics of Deterministic Protein Motion journal, May 1994

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

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

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

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

Crystallography on a chip journal, February 2012

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

Automated data collection for macromolecular crystallography journal, September 2011

Breaking the indexing ambiguity in serial crystallography journal, December 2013

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

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

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

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

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

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

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

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

Overview of the CCP4 suite and current developments. text, January 2011

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

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

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

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

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

Serial protein crystallography in an electron microscope journal, February 2020

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

Microfluidics: From crystallization to serial time-resolved crystallography journal, May 2017

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

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

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

Stable sample delivery in viscous media via a capillary for serial crystallography journal, February 2020

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

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 serial oscillation crystallography at room temperature journal, February 2019

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

Toward G protein-coupled receptor structure-based drug design using X-ray lasers journal, October 2019

A fixed-target platform for serial femtosecond crystallography in a hydrated environment journal, January 2020

Where is crystallography going? journal, February 2018

Resolving polymorphs and radiation-driven effects in microcrystals using fixed-target serial synchrotron crystallography journal, November 2018

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Sample delivery for serial crystallography at free-electron lasers and synchrotrons journal, January 2019

Strategies for sample delivery for femtosecond crystallography journal, February 2019

In situ crystallography as an emerging method for structure solution of membrane proteins: the case of CCR2A journal, November 2019

Serial Femtosecond Crystallography text, January 2015

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

Short-wavelength free-electron laser sources and science: a review text, January 2017

The hit-and-return system enables efficient time-resolved serial synchrotron crystallography text, January 2018

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

Recent Advances in Ultrafast Structural Techniques journal, April 2019

Sample Delivery Media for Serial Crystallography journal, March 2019

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

Energetics and Dynamics of Deterministic Protein Motion
journal, May 1994

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

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

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

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

Crystallography on a chip
journal, February 2012

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

Automated data collection for macromolecular crystallography
journal, September 2011

Breaking the indexing ambiguity in serial crystallography
journal, December 2013

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

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

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

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

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

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

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

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

Overview of the CCP4 suite and current developments.
text, January 2011

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

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

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

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

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

Serial protein crystallography in an electron microscope
journal, February 2020

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

Microfluidics: From crystallization to serial time-resolved crystallography
journal, May 2017

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

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

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

Stable sample delivery in viscous media via a capillary for serial crystallography
journal, February 2020

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

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 serial oscillation crystallography at room temperature
journal, February 2019

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

Toward G protein-coupled receptor structure-based drug design using X-ray lasers
journal, October 2019

A fixed-target platform for serial femtosecond crystallography in a hydrated environment
journal, January 2020

Where is crystallography going?
journal, February 2018

Resolving polymorphs and radiation-driven effects in microcrystals using fixed-target serial synchrotron crystallography
journal, November 2018

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

Sample delivery for serial crystallography at free-electron lasers and synchrotrons
journal, January 2019

Strategies for sample delivery for femtosecond crystallography
journal, February 2019

In situ crystallography as an emerging method for structure solution of membrane proteins: the case of CCR2A
journal, November 2019

Serial Femtosecond Crystallography
text, January 2015

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

Short-wavelength free-electron laser sources and science: a review
text, January 2017

The hit-and-return system enables efficient time-resolved serial synchrotron crystallography
text, January 2018

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

Recent Advances in Ultrafast Structural Techniques
journal, April 2019

Sample Delivery Media for Serial Crystallography
journal, March 2019

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

A fixed-target platform for serial femtosecond crystallography in a hydrated environment
text, January 2020

Serial protein crystallography in an electron microscope
text, January 2020

The hit-and-return system enables efficient time-resolved serial synchrotron crystallography
journal, October 2018