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Crystals
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Advances in Synchrotron Radiation Applications for Crystal Structure Studies
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Advances in Synchrotron Radiation Applications for Crystal Structure Studies

A special issue of Crystals (ISSN 2073-4352). This special issue belongs to the section "Crystal Engineering".

Deadline for manuscript submissions: closed (30 September 2017) | Viewed by 46356

Special Issue Editor

Prof. Dr. William Clegg

E-Mail Website
Guest Editor
School of Natural and Environmental Sciences, Newcastle University, Newcastle upon Tyne, UK
Interests: synchrotron radiation; chemical crystallography; single-crystal X-ray diffraction; crystallographic teaching; structural chemistry; main-group coordination chemistry
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

Crystal structure determination using X-rays is a well-established mature discipline with important applications in chemistry, physics, biology, environmental science, materials science, medicine, and engineering. It brings together scientists from a wide range of research areas, and is generally regarded as the most definitive and exhaustive form of experimental structural characterisation. Recent years have seen major enhancements in aspects of hardware and software, greatly extending the scope and power of the technique. Possibly, the greatest changes have been seen in X-ray detector technology with the widespread introduction since the 1990s of successive types of area detectors, giving advantages in speed, sensitivity and accuracy.

X-ray source developments in the local laboratory have also been important, with improvements in intensity, stability, and the use of advanced X-ray optics. However, much greater enhancements are achieved by carrying out data collection at a storage-ring synchrotron source. This brings advantages, not only in X-ray intensity (up to several orders of magnitude), but also in beam focusing and collimation, in wavelength selection for various purposes, and potentially in exploitation of the pulsed time-structure of the incident X-ray beam. Most of these advantages have been recognised and exploited for decades by biological macromolecular crystallography researchers, but have become generally available in chemical and materials science areas only in the last 20 years. Today, numerous synchrotron beamlines offer single-crystal diffraction capabilities for so-called ‘small molecule’ applications, though only a very few are dedicated to such applications rather than being shared with other diffraction and/or spectroscopic techniques. Nevertheless, there is a growing output of synchrotron-derived crystal structures, not only of relatively stable materials but also of transient and excited states through the emerging technique of photocrystallography. Both the facilities themselves and the uses to which they are put are undergoing significant development.

This Special Issue provides a forum for reports on technical developments and their applications, and for novel research in areas of crystallography that depend on, or benefit from, the use of synchrotron facilities. Scientists working in a wide range of disciplines are invited to contribute to this collection. The topics presented in the keywords cover broadly the focus of this Special Issue, but do not restrict it, as synchrotron applications in crystallography are growing and are likely to include particular approaches that have not yet been described; innovative contributions are particularly welcomed.

Prof. Dr. William Clegg
Guest Editor

Manuscript Submission Information

Manuscripts should be submitted online at www.mdpi.com by registering and logging in to this website. Once you are registered, click here to go to the submission form. Manuscripts can be submitted until the deadline. All submissions that pass pre-check are peer-reviewed. Accepted papers will be published continuously in the journal (as soon as accepted) and will be listed together on the special issue website. Research articles, review articles as well as short communications are invited. For planned papers, a title and short abstract (about 100 words) can be sent to the Editorial Office for announcement on this website.

Submitted manuscripts should not have been published previously, nor be under consideration for publication elsewhere (except conference proceedings papers). All manuscripts are thoroughly refereed through a single-blind peer-review process. A guide for authors and other relevant information for submission of manuscripts is available on the Instructions for Authors page. Crystals is an international peer-reviewed open access monthly journal published by MDPI.

Please visit the Instructions for Authors page before submitting a manuscript. The Article Processing Charge (APC) for publication in this open access journal is 2100 CHF (Swiss Francs). Submitted papers should be well formatted and use good English. Authors may use MDPI's English editing service prior to publication or during author revisions.

Keywords

  • synchrotron crystallography beamlines
  • data collection and processing
  • crystal structures from synchrotron data
  • exploitation of high intensity, focusing and collimation
  • use of wavelength tunability
  • photocrystallography and other time-resolved studies

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Published Papers (6 papers)

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Research

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2455 KiB  
Article
Remote Access Revolution: Chemical Crystallographers Enter a New Era at Diamond Light Source Beamline I19
by Natalie T. Johnson, Paul G. Waddell, William Clegg and Michael R. Probert
Crystals 2017, 7(12), 360; https://doi.org/10.3390/cryst7120360 - 5 Dec 2017
Cited by 28 | Viewed by 6317
Abstract
Since the inception of the use of synchrotron radiation in the structural characterisation of crystalline materials by single-crystal diffraction in the late 20th century, the field has undergone an explosion of technological developments. These cover all aspects of the experiments performed, from the [...] Read more.
Since the inception of the use of synchrotron radiation in the structural characterisation of crystalline materials by single-crystal diffraction in the late 20th century, the field has undergone an explosion of technological developments. These cover all aspects of the experiments performed, from the construction of the storage rings and insertion devices, to the end user functionalities in the experimental hutches. Developments in automation have most frequently been driven by the macromolecular crystallography community. The drive towards greater access to ever-brighter X-ray sources has benefited the entire field. Herein, we detail the revolution that is now occurring within the chemical crystallography community, utilising many of the tools developed by their more biologically oriented colleagues, along with specialised functionalities that are tailored to the small-molecule world. We discuss the benefits of utilising the advanced features of Diamond Light Source beamline I19 in the newly developed remote access mode and the step-change in productivity that can be established as a result. Full article
(This article belongs to the Special Issue Advances in Synchrotron Radiation Applications for Crystal Structure Studies)
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12766 KiB  
Article
A Novel Dual Air-Bearing Fixed-χ Diffractometer for Small-Molecule Single-Crystal X-ray Diffraction on Beamline I19 at Diamond Light Source
by David . R Allan, Harriott Nowell, Sarah A. Barnett, Mark R. Warren, Adrian Wilcox, Jeppe Christensen, Lucy K. Saunders, Andrew Peach, Mark T. Hooper, Ljubo Zaja, Suren Patel, Leo Cahill, Russell Marshall, Steven Trimnell, Andrew J. Foster, Trevor Bates, Simon Lay, Mark A. Williams, Paul V. Hathaway, Graeme Winter, Markus Gerstel and Ron W. Wooleyadd Show full author list remove Hide full author list
Crystals 2017, 7(11), 336; https://doi.org/10.3390/cryst7110336 - 2 Nov 2017
Cited by 57 | Viewed by 11170
Abstract
Herein, we describe the development of a novel dual air-bearing fixed-χ diffractometer for beamline I19 at Diamond Light Source. The diffractometer is designed to facilitate the rapid data collections possible with a Dectris Pilatus 2M pixel-array photon-counting detector, while allowing remote operation in [...] Read more.
Herein, we describe the development of a novel dual air-bearing fixed-χ diffractometer for beamline I19 at Diamond Light Source. The diffractometer is designed to facilitate the rapid data collections possible with a Dectris Pilatus 2M pixel-array photon-counting detector, while allowing remote operation in conjunction with a robotic sample changer. The sphere-of-confusion is made as small as practicably possible, through the use of air-bearings for both the ω and φ axes. The design and construction of the new instrument is described in detail and an accompanying paper by Johnson et al. (also in this issue) will provide a user perspective of its operation. Full article
(This article belongs to the Special Issue Advances in Synchrotron Radiation Applications for Crystal Structure Studies)
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3701 KiB  
Article
High-Throughput Small-Molecule Crystallography at the ‘Belok’ Beamline of the Kurchatov Synchrotron Radiation Source: Transition Metal Complexes with Azomethine Ligands as a Case Study
by Vladimir A. Lazarenko, Pavel V. Dorovatovskii, Yan V. Zubavichus, Anatolii S. Burlov, Yurii V. Koshchienko, Valery G. Vlasenko and Victor N. Khrustalev
Crystals 2017, 7(11), 325; https://doi.org/10.3390/cryst7110325 - 28 Oct 2017
Cited by 110 | Viewed by 7599
Abstract
This paper concisely describes capabilities of the ‘Belok’ beamline at the Kurchatov synchrotron radiation source, related to high-throughput small-molecule X-ray crystallography. As case examples, a series of four novel transition metal complexes with azomethine ligands were selected. The complexes demonstrate somewhat unexpected changes [...] Read more.
This paper concisely describes capabilities of the ‘Belok’ beamline at the Kurchatov synchrotron radiation source, related to high-throughput small-molecule X-ray crystallography. As case examples, a series of four novel transition metal complexes with azomethine ligands were selected. The complexes demonstrate somewhat unexpected changes in the coordination geometry and nuclearity in response to the introduction of substituents in the ligand’s periphery. Full article
(This article belongs to the Special Issue Advances in Synchrotron Radiation Applications for Crystal Structure Studies)
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3156 KiB  
Article
Synchrotron Radiation Pair Distribution Function Analysis of Gels in Cements
by Ana Cuesta, Jesus D. Zea-Garcia, Diana Londono-Zuluaga, Angeles G. De la Torre, Isabel Santacruz, Oriol Vallcorba and Miguel A.G. Aranda
Crystals 2017, 7(10), 317; https://doi.org/10.3390/cryst7100317 - 18 Oct 2017
Cited by 20 | Viewed by 5786
Abstract
The analysis of atomic ordering in a nanocrystalline phase with small particle sizes, below 5 nm, is intrinsically complicated because of the lack of long-range order. Furthermore, the presence of additional crystalline phase(s) may exacerbate the problem, as is the case in cement [...] Read more.
The analysis of atomic ordering in a nanocrystalline phase with small particle sizes, below 5 nm, is intrinsically complicated because of the lack of long-range order. Furthermore, the presence of additional crystalline phase(s) may exacerbate the problem, as is the case in cement pastes. Here, we use the synchrotron pair distribution function (PDF) chiefly to characterize the local atomic order of the nanocrystalline phases, gels, in cement pastes. We have used a multi r-range analysis approach, where the ~4–7 nm r-range allows determining the crystalline phase contents; the ~1–2.5 nm r-range is used to characterize the atomic ordering in the nanocrystalline component; and the ~0.2–1.0 nm r-range gives insights about additional amorphous components. Specifically, we have prepared four alite pastes with variable water contents, and the analyses showed that a defective tobermorite, Ca11Si9O28(OH)2.8.5H2O, gave the best fit. Furthermore, the PDF analyses suggest that the calcium silicate hydrate gel is composed of this tobermorite and amorphous calcium hydroxide. Finally, this approach has been used to study alternative cements. The hydration of monocalcium aluminate and ye’elimite pastes yield aluminum hydroxide gels. PDF analyses show that these gels are constituted of nanocrystalline gibbsite, and the particle size can be as small as 2.5 nm. Full article
(This article belongs to the Special Issue Advances in Synchrotron Radiation Applications for Crystal Structure Studies)
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2217 KiB  
Article
Structure of a Novel Spinel Li0.5Zn5/3Sb2.5/3O4 by Neutron and Synchrotron Diffraction Analysis
by José Alfredo Marín-Romero, Luis Edmundo Fuentes-Cobas, Juan Rodríguez-Carvajal, Carolina Tabasco-Novelo and Patricia Quintana
Crystals 2017, 7(9), 280; https://doi.org/10.3390/cryst7090280 - 15 Sep 2017
Cited by 5 | Viewed by 7314
Abstract
Zn7/3Sb2/3O4 is a secondary phase in ZnO-based varistors. Acceptor impurities, such as Li+, increase the resistivity. This effect is produced by a modification of the grain boundary barriers. The role of the cationic distribution in the [...] Read more.
Zn7/3Sb2/3O4 is a secondary phase in ZnO-based varistors. Acceptor impurities, such as Li+, increase the resistivity. This effect is produced by a modification of the grain boundary barriers. The role of the cationic distribution in the mentioned events is worth clarifying. The Li0.5Zn5/3Sb2.5/3O4 room-temperature structure was determined by means of a neutron diffraction and synchrotron X-ray diffraction investigation. The title compound was prepared by conventional ceramic process. The elemental composition of the investigated sample was verified by means of electron microscopy—energy dispersive X-ray spectroscopy and X-ray photoelectron spectroscopy. The neutron experiment was performed at the high-intensity neutron diffractometer with position-sensitive detector at the D1B beamline of the Laue-Langevin Institute, Grenoble. The high resolution synchrotron measurement was carried out at MCX beamline of Elettra Sincrotrone Trieste. Rietveld analysis was performed with the FullProf program. Li0.5Zn5/3Sb2.5/3O4 belongs to the spinel family, space group F d 3 ¯ m (227). The measured lattice parameter is a = 8.5567(1) Å. The Li+1 and Zn+2 ions are randomly distributed among the tetrahedral and octahedral sites as opposed to Sb+5 ions which have preference for octahedral sites. Fractional coordinate of oxygen, u = 0.2596(1), indicates a slight deformation of the tetrahedral and octahedral sites. The data given in this paper provide structural support for further studies on measurements and microscopic explanations of the interesting properties of this family of compounds. Full article
(This article belongs to the Special Issue Advances in Synchrotron Radiation Applications for Crystal Structure Studies)
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Review

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18898 KiB  
Review
Chemical Crystallography at the Advanced Light Source
by Laura J. McCormick, Nico Giordano, Simon J. Teat and Christine M. Beavers
Crystals 2017, 7(12), 382; https://doi.org/10.3390/cryst7120382 - 18 Dec 2017
Cited by 6 | Viewed by 6818
Abstract
Chemical crystallography at synchrotrons was pioneered at the Daresbury SRS station 9.8. The chemical crystallography beamlines at the Advanced Light Source seek to follow that example, with orders of magnitude more flux than a lab source, and various in situ experiments. This article [...] Read more.
Chemical crystallography at synchrotrons was pioneered at the Daresbury SRS station 9.8. The chemical crystallography beamlines at the Advanced Light Source seek to follow that example, with orders of magnitude more flux than a lab source, and various in situ experiments. This article attempts to answer why a chemist would require synchrotron X-rays, to describe the techniques available at the ALS chemical crystallography beamlines, and place the current facilities in a historical context. Full article
(This article belongs to the Special Issue Advances in Synchrotron Radiation Applications for Crystal Structure Studies)
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