scholarly journals Kilohertz Macromolecular Crystallography Using an EIGER Detector at Low X-ray Fluxes

Crystals ◽  
2020 ◽  
Vol 10 (12) ◽  
pp. 1146
Author(s):  
Krishna P. Khakurel ◽  
Shirly Espinoza ◽  
Martin Savko ◽  
Vitaly Polovinkin ◽  
Jan Dohnalek ◽  
...  
Keyword(s):  
Frame Rate ◽  
Macromolecular Crystallography ◽  
Experimental Proof ◽  
Time Resolved ◽  
X Ray ◽  
High Repetition ◽  
Pixel Detectors ◽  
Low X ◽  
Significant Effort ◽  
Made In

Time-resolved in-house macromolecular crystallography is primarily limited by the capabilities of the in-house X-ray sources. These sources can only provide a time-averaged structure of the macromolecules. A significant effort has been made in the development of in-house laser-driven ultrafast X-ray sources, with one of the goals as realizing the visualization of the structural dynamics of macromolecules at a very short timescale within the laboratory-scale infrastructure. Most of such in-house ultrafast X-ray sources are operated at high repetition rates and usually deliver very low flux. Therefore, the necessity of a detector that can operate at the repetition rate of the laser and perform extremely well under low flux conditions is essential. Here, we present experimental results demonstrating the usability of the hybrid-pixel detectors, such as Eiger X 1M, and provide experimental proof that they can be successfully operated to collect macromolecular crystallographic data up to a detector frame rate of 3 kHz from synchrotron sources. Our results also show that the data reduction and structural analysis are successful at such high frame rates and fluxes as low as 108 photons/s, which is comparable to the values expected from a typical laser-driven X-ray source.

scholarly journals Automated harvesting and processing of protein crystals through laser photoablation

2016 ◽  
Vol 72 (4) ◽  
pp. 454-466 ◽  
Author(s):  
Ulrich Zander ◽  
Guillaume Hoffmann ◽  
Irina Cornaciu ◽  
Jean-Pierre Marquette ◽  
Gergely Papp ◽  
...  
Keyword(s):  
Data Collection ◽  
Macromolecular Crystallography ◽  
X Ray Diffraction ◽  
X Ray ◽  
New Methods ◽  
Repeated Sample ◽  
Sample Recovery ◽  
Through Diffusion ◽  
X Ray Background ◽  
Low X

Currently, macromolecular crystallography projects often require the use of highly automated facilities for crystallization and X-ray data collection. However, crystal harvesting and processing largely depend on manual operations. Here, a series of new methods are presented based on the use of a low X-ray-background film as a crystallization support and a photoablation laser that enable the automation of major operations required for the preparation of crystals for X-ray diffraction experiments. In this approach, the controlled removal of the mother liquor before crystal mounting simplifies the cryocooling process, in many cases eliminating the use of cryoprotectant agents, while crystal-soaking experiments are performed through diffusion, precluding the need for repeated sample-recovery and transfer operations. Moreover, the high-precision laser enables new mounting strategies that are not accessible through other methods. This approach bridges an important gap in automation and can contribute to expanding the capabilities of modern macromolecular crystallography facilities.

scholarly journals New ASCA Observations of two Anomalous X-ray Pulsars

2000 ◽  
Vol 177 ◽  
pp. 695-698 ◽  
Author(s):  
B. Paul ◽  
M. Kawasaki ◽  
T. Dotani ◽  
F. Nagase
Keyword(s):  
Accretion Rate ◽  
Accretion Disc ◽  
Spectral Shape ◽  
Energy Spectra ◽  
Pulse Profile ◽  
X Ray ◽  
Low Mass ◽  
Low X ◽  
Star Surface ◽  
Made In

AbstractNewASCAobservations of two anomalous X-ray pulsars (AXP) 4U 0142+61 and 1E 1048.1-5937, made in 1998, when compared to earlier observations in 1994 show remarkable stability in the intensity, spectral shape and pulse profile. The energy spectra consist of two components, a power-law and a blackbody emission from the neutron star surface. In IE 1048.1-5937, we have identified three epochs with different spin-down rates and discuss its implications for the magnetar hypothesis of the AXPs. We also note that the spin-down rate and its variations in IE 1048.1-5937 are much larger than what normally can be produced by an accretion disc with very low mass accretion rate corresponding to its low X-ray luminosity.

scholarly journals Time-Resolved Macromolecular Crystallography at Pulsed X-ray Sources

2019 ◽  
Vol 20 (6) ◽  
pp. 1401 ◽  
Author(s):  
Marius Schmidt
Keyword(s):  
Structural Biology ◽  
Free Electron ◽  
Reaction Dynamics ◽  
X Rays ◽  
Free Electron Lasers ◽  
Macromolecular Crystallography ◽  
Time Resolved ◽  
X Ray ◽  
Methodological Aspects

The focus of structural biology is shifting from the determination of static structures to the investigation of dynamical aspects of macromolecular function. With time-resolved macromolecular crystallography (TRX), intermediates that form and decay during the macromolecular reaction can be investigated, as well as their reaction dynamics. Time-resolved crystallographic methods were initially developed at synchrotrons. However, about a decade ago, extremely brilliant, femtosecond-pulsed X-ray sources, the free electron lasers for hard X-rays, became available to a wider community. TRX is now possible with femtosecond temporal resolution. This review provides an overview of methodological aspects of TRX, and at the same time, aims to outline the frontiers of this method at modern pulsed X-ray sources.

RADDOSE-3D: time- and space-resolved modelling of dose in macromolecular crystallography

2013 ◽  
Vol 46 (4) ◽  
pp. 1225-1230 ◽  
Author(s):  
Oliver B. Zeldin ◽  
Markus Gerstel ◽  
Elspeth F. Garman
Keyword(s):  
Data Collection ◽  
Radiation Damage ◽  
Diffraction Experiment ◽  
Macromolecular Crystallography ◽  
X Ray Diffraction ◽  
Time Resolved ◽  
X Ray ◽  
Online Methods ◽  
Crystal Volume ◽  
Number Of Iterations

RADDOSE-3D allows the macroscopic modelling of an X-ray diffraction experiment for the purpose of better predicting radiation-damage progression. The distribution of dose within the crystal volume is calculated for a number of iterations in small angular steps across one or more data collection wedges, providing a time-resolved picture of the dose state of the crystal. The code is highly modular so that future contributions from the community can be easily integrated into it, in particular to incorporate online methods for determining the shape of macromolecular crystals and better protocols for imaging real experimental X-ray beam profiles.

A new family of pixel detectors for high frame rate X-ray applications

2010 ◽  
Vol 617 (1-3) ◽  
pp. 384-386 ◽  
Author(s):  
Roberto Dinapoli ◽  
Anna Bergamaschi ◽  
Beat Henrich ◽  
Roland Horisberger ◽  
Ian Johnson ◽  
...  
Keyword(s):  
Frame Rate ◽  
X Ray ◽  
High Frame Rate ◽  
New Family ◽  
Pixel Detectors

Crystallization Characteristics of Ge-Sb Phase Change Materials

2009 ◽  
Vol 1160 ◽  
Author(s):  
Simone Raoux ◽  
Cyril Cabral ◽  
Lia Krusin-Elbaum ◽  
Jean L. Jordan-Sweet ◽  
Martin Salinga ◽  
...  
Keyword(s):  
Phase Change ◽  
Phase Change Materials ◽  
Mass Density ◽  
Large Change ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Time Resolved ◽  
X Ray ◽  
Diffraction Peaks ◽  
Low X

AbstractThe crystallization behavior of Ge-Sb phase change materials with variable Ge:Sb ratio X between 0.079 and 4.3 was studied using time-resolved x-ray diffraction, differential scanning calorimetry, x-ray reflectivity, optical reflectivity and resistivity vs. temperature measurements. It was found that the crystallization temperature increases with Ge content from about 130 °C for X = 0.079 to about 450 °C for X = 4.3. For low X, Sb x-ray diffraction peaks occurred during a heating ramp at lower temperature than Ge diffraction peaks. For X = 1.44 and higher, Sb and Ge peaks occurred at the same temperature. Mass density change upon crystallization and optical and electrical contrast between the phases show a maximum for the eutectic alloy with X = 0.17. The large change in materials properties with composition allows tailoring of the crystallization properties for specific application requirements.

Time-resolved macromolecular crystallography: introductory remarks and a little history

1992 ◽  
Vol 340 (1657) ◽  
pp. 169-173 ◽  
Keyword(s):  
Crystallographic Data ◽  
Macromolecular Crystallography ◽  
Time Resolved ◽  
X Ray ◽  
Early Use ◽  
Laue Method

X -ray crystallographic data can be collected rapidly at synchrotrons by the Laue method. The early use of the Laue method by Ewald, Nishikawa, Wyckoff and Pauling is reviewed.

scholarly journals 3D-MiXD: 3D-printed X-ray-compatible microfluidic devices for rapid, low-consumption serial synchrotron crystallography data collection in flow

IUCrJ ◽  
2020 ◽  
Vol 7 (2) ◽  
pp. 207-219 ◽  
Author(s):  
Diana C. F. Monteiro ◽  
David von Stetten ◽  
Claudia Stohrer ◽  
Marta Sans ◽  
Arwen R. Pearson ◽  
...  
Keyword(s):  
Data Collection ◽  
Room Temperature ◽  
Time Resolved ◽  
X Ray ◽  
Biologically Relevant ◽  
3D Printed ◽  
Serial Crystallography ◽  
Low X ◽  
Very High

Serial crystallography has enabled the study of complex biological questions through the determination of biomolecular structures at room temperature using low X-ray doses. Furthermore, it has enabled the study of protein dynamics by the capture of atomically resolved and time-resolved molecular movies. However, the study of many biologically relevant targets is still severely hindered by high sample consumption and lengthy data-collection times. By combining serial synchrotron crystallography (SSX) with 3D printing, a new experimental platform has been created that tackles these challenges. An affordable 3D-printed, X-ray-compatible microfluidic device (3D-MiXD) is reported that allows data to be collected from protein microcrystals in a 3D flow with very high hit and indexing rates, while keeping the sample consumption low. The miniaturized 3D-MiXD can be rapidly installed into virtually any synchrotron beamline with only minimal adjustments. This efficient collection scheme in combination with its mixing geometry paves the way for recording molecular movies at synchrotrons by mixing-triggered millisecond time-resolved SSX.

Sign in / Sign up

Export Citation Format

Share Document