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In‐house time‐resolved photocrystallography on the millisecond timescale using a gated X‐ray hybrid pixel area detector
Author(s) -
Casaretto Nicolas,
Schaniel Dominik,
Alle Paul,
Wenger Emmanuel,
Parois Pascal,
Fournier Bertrand,
Bendeif El-Eulmi,
Palin Cyril,
Pillet Sébastien
Publication year - 2017
Publication title -
acta crystallographica section b
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.604
H-Index - 33
ISSN - 2052-5206
DOI - 10.1107/s2052520617009234
Subject(s) - femtosecond , diffraction , optics , detector , laser , millisecond , shutter , diffractometer , materials science , physics , scanning electron microscope , astronomy
With the remarkable progress of accelerator‐based X‐ray sources in terms of intensity and brightness, the investigation of structural dynamics from time‐resolved X‐ray diffraction methods is becoming widespread in chemistry, biochemistry and materials science applications. Diffraction patterns can now be measured down to the femtosecond time‐scale using X‐ray free electron lasers or table‐top laser plasma X‐ray sources. On the other hand, the recent developments in photon counting X‐ray area detectors offer new opportunities for time‐resolved crystallography. Taking advantage of the fast read‐out, the internal stacking of recorded images, and the gating possibilities (electronic shutter) of the XPAD hybrid pixel detector, we implemented a laboratory X‐ray diffractometer for time‐resolved single‐crystal X‐ray diffraction after pulsed laser excitation, combined with transient optical absorption measurement. The experimental method and instrumental setup are described in detail, and validated using the photoinduced nitrosyl linkage isomerism of sodium nitroprusside, Na 2 [Fe(CN) 5 NO]·2H 2 O, as proof of principle. Light‐induced Bragg intensity relative variations Δ I ( hkl )/ I ( hkl ) of the order of 1%, due to the photoswitching of the NO ligand, could be detected with a 6 ms acquisition window. The capabilities of such a laboratory time‐resolved experiment are critically evaluated.