Pump–probe capabilities at the SPB/SFX instrument of the European XFEL

Koliyadu, Jayanath; Letrun, Romain; Kirkwood, Henry; Liu, Jia; Jiang, Ming; Emons, Moritz; Bean, Richard; Bellucci, Valerio; Bielecki, Johan; Birnšteinová, Šarlota; Wijn, Raphaël de; Dietze, Thomas; Juncheng, E; Grünert, Jan; Kane, Daniel; Kim, Chan; Kim, Yoonhee; Lederer, Max; Manning, Bradley C.; Mills, Grant; Morillo, Luis López; Reimers, Nadja; Rompotis, Dimitrios; Round, Adam; Sikorski, Marcin; Takem, Cedric M. S.; Vagovič, Patrik; Venkatesan, Sandhya; Wang, Jinxiong; Wegner, U.; Mancuso, Adrian P.; Sato, Tokushi

doi:10.1107/s1600577522006701

Cited by 14 publications

(7 citation statements)

References 45 publications

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“…OaPAC microcrystals were photoexcited with the second harmonic of the EuXFEL pump—probe laser system 82–84 at 421 nm. The optical pump pulses were stretched from their original duration of 50 fs to 250 fs by transmission through fused silica.…”

Section: Methodsmentioning

confidence: 99%

“…The microcrystal slurry was concentrated to 20% pellet volume (v/v) after sedimentation. The slurry was injected with a gas dynamic virtual nozzle (GDVN) 80 for a serial femtosecond crystallography (SFX) experiment at the SPB/SFX instrument 81 OaPAC microcrystals were photoexcited with the second harmonic of the EuXFEL pump-probe laser system [82][83][84] at 421 nm. The optical pump pulses were stretched from their original duration of 50 fs to 250 fs by transmission through fused silica.…”

Section: Microcrystals Growth and Tr-sfx Experimentsmentioning

confidence: 99%

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Light-induced Trpin/Metout switching during BLUF domain activation in ATP-bound photoactivatable adenylate cyclase OaPAC

Chretien,

Nagel,

Botha

et al. 2023

Preprint

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The understanding of signal transduction mechanisms in photoreceptor proteins is essential for elucidating how living organisms respond to light as environmental stimuli. In this study, we investigated the ATP binding, photoactivation and signal transduction process in the photoactivatable adenylate cyclase from Oscillatoria acuminata (OaPAC) upon blue light excitation. Structural models with ATP bound in the active site of native OaPAC at cryogenic as well as room temperature are presented. ATP is found in one conformation at cryogenic- and in two conformations at ambient-temperature, and is bound in a non-productive conformation. However, FTIR spectroscopic experiments confirm that the non-productive conformation is the native binding mode in dark state OaPAC and that transition to a productive conformation for ATP turnover only occurs after light activation. A combination of time-resolved crystallography experiments at synchrotron and X-ray Free Electron Lasers sheds light on the initial events around the Flavin Adenine Dinucleotide (FAD) chromophore in the light-sensitive BLUF domain of OaPAC. Initial changes involve the highly conserved amino acids Tyr6, Gln48 and Met92. Crucially, the Gln48 side chain performs a 180 degree rotation during activation, leading to the stabilization of the FAD chromophore. Cryo-trapping experiments allowed us to investigate a late light-activated state of the reaction and revealed significant conformational changes in the BLUF domain around the FAD chromophore. In particular, a Trpin/Metout transition upon illumination is observed for the first time in the BLUF domain and its role in signal transmission via alpha-helix 3 and 4 in the linker region between sensor and effector domain is discussed.

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Section: Methodsmentioning

confidence: 99%

Section: Microcrystals Growth and Tr-sfx Experimentsmentioning

confidence: 99%

Light-induced Trpin/Metout switching during BLUF domain activation in ATP-bound photoactivatable adenylate cyclase OaPAC

Chretien,

Nagel,

Botha

et al. 2023

Preprint

Self Cite

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“…Alignment of the nozzle tip with respect to the interaction region was carried out by manipulating the position of the injector rod using motorized stages. This placement was aided by visualization with the side view microscope camera illuminated with the EuXFEL femtosecond laser coupled into the sample chamber via a fiber bundle laser synchronized with the X-ray pulse (Koliyadu et al, 2022;Palmer et al, 2019).…”

Section: Liquid Sample Injection At Euxfel Spb/sfxmentioning

confidence: 99%

3D-printed sheet jet for stable megahertz liquid sample delivery at X-ray free-electron lasers

Konold,

You,

Bielecki

et al. 2023

IUCrJ

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X-ray free-electron lasers (XFELs) can probe chemical and biological reactions as they unfold with unprecedented spatial and temporal resolution. A principal challenge in this pursuit involves the delivery of samples to the X-ray interaction point in such a way that produces data of the highest possible quality and with maximal efficiency. This is hampered by intrinsic constraints posed by the light source and operation within a beamline environment. For liquid samples, the solution typically involves some form of high-speed liquid jet, capable of keeping up with the rate of X-ray pulses. However, conventional jets are not ideal because of radiation-induced explosions of the jet, as well as their cylindrical geometry combined with the X-ray pointing instability of many beamlines which causes the interaction volume to differ for every pulse. This complicates data analysis and contributes to measurement errors. An alternative geometry is a liquid sheet jet which, with its constant thickness over large areas, eliminates the problems related to X-ray pointing. Since liquid sheets can be made very thin, the radiation-induced explosion is reduced, boosting their stability. These are especially attractive for experiments which benefit from small interaction volumes such as fluctuation X-ray scattering and several types of spectroscopy. Although their use has increased for soft X-ray applications in recent years, there has not yet been wide-scale adoption at XFELs. Here, gas-accelerated liquid sheet jet sample injection is demonstrated at the European XFEL SPB/SFX nano focus beamline. Its performance relative to a conventional liquid jet is evaluated and superior performance across several key factors has been found. This includes a thickness profile ranging from hundreds of nanometres to 60 nm, a fourfold increase in background stability and favorable radiation-induced explosion dynamics at high repetition rates up to 1.13 MHz. Its minute thickness also suggests that ultrafast single-particle solution scattering is a possibility.

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“…To measure experimentally this time shift, the use of a synchrotron pulsed X-ray source is necessary. Pump-probe techniques are commonly employed to achieve nanosecond time resolution (Rehn et al, 1990;Koliyadu et al, 2022). Very often, a laser is used as pump and the specimen is probed by X-rays in many scientific domains such as biology (Berera et al, 2009), chemistry (Britz et al, 2016), physics (Laulhe ´et al, 2012;Silly et al, 2017) and materials science (Gonzalez Vallejo, 2019).…”

Section: Introductionmentioning

confidence: 99%

Investigation of the mechanical work during ultrasonic fatigue loading using pulsed time-resolved X-ray diffraction

Jacquemain,

Cheuleu,

Ranc

et al. 2024

J Synchrotron Radiat

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In the energy production and transportation industries, numerous metallic structures may be subjected to at least several billions of cycles, i.e. loaded in the very high cycle fatigue domain (VHCF). Therefore, to design structures in the VHCF domain, a reliable methodology is necessary. One useful quantity to characterize plastic activity at the microscopic scale and fatigue damage evolution is the mechanical work supplied to a material. However, the estimation of this mechanical work in a metal during ultrasonic fatigue tests remains challenging. This paper aims to present an innovative methodology to quantify this. An experimental procedure was developed to estimate the mechanical work from stress and total strain evolution measurements during one loading cycle with a time accuracy of about 50 ns. This was achieved by conducting time-resolved X-ray diffraction coupled to strain gauge measurements at a synchrotron facility working in pulsed mode (single-bunch mode).

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Pump–probe capabilities at the SPB/SFX instrument of the European XFEL

Cited by 14 publications

References 45 publications

Light-induced Trpin/Metout switching during BLUF domain activation in ATP-bound photoactivatable adenylate cyclase OaPAC

Light-induced Trpin/Metout switching during BLUF domain activation in ATP-bound photoactivatable adenylate cyclase OaPAC

3D-printed sheet jet for stable megahertz liquid sample delivery at X-ray free-electron lasers

Investigation of the mechanical work during ultrasonic fatigue loading using pulsed time-resolved X-ray diffraction

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