Combining on-line spectroscopy with synchrotron and X-ray free electron laser crystallography

Makita, Hiroki; Simon, Philipp S.; Kern, Jan; Yano, Junko; Yachandra, Vittal K.

doi:10.1016/j.sbi.2023.102604

Cited by 4 publications

(10 citation statements)

References 48 publications

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“…The multimodal method of crystallography and XES at XFEL was initially developed for the light-driven water oxidation reaction in PS II, in which the catalytic center consists of Mn (see Section ). Now it is more broadly used for various metalloenzyme studies, by collecting Kα and Kβ 1,3 XES of Mn, Fe, and Ni. , This approach empowers the interpretation of catalytic processes, through the combination of structural information on the protein and chemical information on the metal catalytic center under the exact same experimental conditions. The example of the PS II study is described in detail in Section .…”

Section: Emerging Time-resolved In Situ/operando X-ray Methodsmentioning

confidence: 99%

“…A similar approach can be used at XFELs for studying photochemical reactions of enzymes and molecular charge transfer systems (Figure 11e). 67,68,65 The XES method has often been used together with X-ray diffraction methods (see Figure 6a) and has become a powerful approach to bridge geometric and electronic structural changes. As the same incident X-ray energy can be used for both measurements, the method can track the redox state of metal catalytic centers of metalloproteins during crystallography.…”

Section: X-ray Emission Spectroscopy (Xes)mentioning

confidence: 99%

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Deciphering Photoinduced Catalytic Reaction Mechanisms in Natural and Artificial Photosynthetic Systems on Multiple Temporal and Spatial Scales Using X-ray Probes

Chen,

Yano

2024

Chem. Rev.

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Section: Emerging Time-resolved In Situ/operando X-ray Methodsmentioning

confidence: 99%

Section: X-ray Emission Spectroscopy (Xes)mentioning

confidence: 99%

Deciphering Photoinduced Catalytic Reaction Mechanisms in Natural and Artificial Photosynthetic Systems on Multiple Temporal and Spatial Scales Using X-ray Probes

Chen,

Yano

2024

Chem. Rev.

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“…Performing these experiments without prior knowledge could prove to be very time-consuming both for data acquisition and analysis. For experiments on coloured proteins, UV-Vis absorption spectroscopy appears to be a suitable complementary technique to rapidly provide information on successful cryo-trapping strategies or time points of particular interest by identifying intermediates with specific spectroscopic signatures (von Stetten et al, 2015;Makita et al, 2023).…”

Section: How To Monitor the Progress Of A Reaction Within The Crystalmentioning

confidence: 99%

From femtoseconds to minutes: time-resolved macromolecular crystallography at XFELs and synchrotrons

Caramello,

Royant

2024

Acta Crystallogr D Struct Biol

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Over the last decade, the development of time-resolved serial crystallography (TR-SX) at X-ray free-electron lasers (XFELs) and synchrotrons has allowed researchers to study phenomena occurring in proteins on the femtosecond-to-minute timescale, taking advantage of many technical and methodological breakthroughs. Protein crystals of various sizes are presented to the X-ray beam in either a static or a moving medium. Photoactive proteins were naturally the initial systems to be studied in TR-SX experiments using pump–probe schemes, where the pump is a pulse of visible light. Other reaction initiations through small-molecule diffusion are gaining momentum. Here, selected examples of XFEL and synchrotron time-resolved crystallography studies will be used to highlight the specificities of the various instruments and methods with respect to time resolution, and are compared with cryo-trapping studies.

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“…Three examples stand out. (1) The "in situ" monitoring of radiative damage in X-ray experiments, 93,94 (2) providing a fast response operando spectroscopy dimension to kinetic measurements with online MS or GC analysis (e.g., TAP, SSITKA, step response), 95−98 and (3) selectively probing specific absorption features which we elaborate on further. The complementary information derived from the coupled techniques enables site-selective spectroscopy, where the spectroscopic data are unambiguously linked to the same UV−vis−NIR absorption band.…”

Section: Coupling To Complementary Techniquesmentioning

confidence: 99%

“…Three examples stand out. (1) The “ in situ ” monitoring of radiative damage in X-ray experiments, , (2) providing a fast response operando spectroscopy dimension to kinetic measurements with online MS or GC analysis (e.g., TAP, SSITKA, step response), − and (3) selectively probing specific absorption features which we elaborate on further.…”

Section: Role Of In Situ Uv–vis–nir Absorption Spectroscopiesmentioning

confidence: 99%

In Situ UV–Vis–NIR Absorption Spectroscopy and Catalysis

Bols,

Ma,

Rammal

et al. 2024

Chem. Rev.

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This review highlights in situ UV–vis–NIR range absorption spectroscopy in catalysis. A variety of experimental techniques identifying reaction mechanisms, kinetics, and structural properties are discussed. Stopped flow techniques, use of laser pulses, and use of experimental perturbations are demonstrated for in situ studies of enzymatic, homogeneous, heterogeneous, and photocatalysis. They access different time scales and are applicable to different reaction systems and catalyst types. In photocatalysis, femto- and nanosecond resolved measurements through transient absorption are discussed for tracking excited states. UV–vis–NIR absorption spectroscopies for structural characterization are demonstrated especially for Cu and Fe exchanged zeolites and metalloenzymes. This requires combining different spectroscopies. Combining magnetic circular dichroism and resonance Raman spectroscopy is especially powerful. A multitude of phenomena can be tracked on transition metal catalysts on various supports, including changes in oxidation state, adsorptions, reactions, support interactions, surface plasmon resonances, and band gaps. Measurements of oxidation states, oxygen vacancies, and band gaps are shown on heterogeneous catalysts, especially for electrocatalysis. UV–vis–NIR absorption is burdened by broad absorption bands. Advanced analysis techniques enable the tracking of coking reactions on acid zeolites despite convoluted spectra. The value of UV–vis–NIR absorption spectroscopy to catalyst characterization and mechanistic investigation is clear but could be expanded.

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Combining on-line spectroscopy with synchrotron and X-ray free electron laser crystallography

Cited by 4 publications

References 48 publications

Deciphering Photoinduced Catalytic Reaction Mechanisms in Natural and Artificial Photosynthetic Systems on Multiple Temporal and Spatial Scales Using X-ray Probes

Deciphering Photoinduced Catalytic Reaction Mechanisms in Natural and Artificial Photosynthetic Systems on Multiple Temporal and Spatial Scales Using X-ray Probes

From femtoseconds to minutes: time-resolved macromolecular crystallography at XFELs and synchrotrons

In Situ UV–Vis–NIR Absorption Spectroscopy and Catalysis

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