A Single-Crystal X-ray Diffractometer for High-Power, High-Throughput Chemical Crystallography
Lead Research Organisation:
University of Sussex
Department Name: Sch of Life Sciences
Abstract
We request support for a state-of-the-art Metaljet single-crystal X-ray diffractometer equipped with an automated robotic sample changer. This equipment will underpin a variety of current research projects in the South-East region of the UK and will enable many more in the future.
X-ray crystallography is the most important technique for determining the structures of crystalline solids. The UK boasts a history of pioneering discovery in crystallography, including several Nobel Prizes. Today, the strength of the research base is such that the UK leads the world in crystallography. The reach and impact of the technique is remarkable, spanning chemistry, life sciences, materials science, condensed matter physics and earth sciences, and incorporating a broad community of industrial and academic users.
The vision for our proposal is to enable rapid structure determination across length scales, from small molecules and supramolecules to chemical-biological systems and extended solids. Examples of these materials include catalysts, molecular magnets, pharmaceutical ingredients, polymers, amphiphiles, drug molecules bound to biological targets, energy materials and metal-organic frameworks. Many of these materials form as very small crystals that are difficult or impossible to measure in full on existing in-house diffractometers, which limits the value of the structural information and acts as a barrier to its downstream implementation. We propose to use striking recent advances in diffraction technology, including the availability of X-ray beams with unprecedentedly high brilliance and detectors with very high sensitivity, that will enable the measurement of such crystals. The resulting information will enable the development of more accurate structure-function relationships for the materials of interest.
The automated robotic sample changer will provide game-changing capability. Conventional approaches to single-crystal measurements can be time-consuming, requiring hands-on effort to mount, centre and measure individual crystals. The robot will allow multiple consecutive measurements of single crystals without the need for human intervention. Automation then allows the quality of the crystals to be ranked and the best one selected for further measurements. This will be of immediate benefit to the majority of the user base, whose samples will be measured in full in Sussex. It will also benefit users with samples that require further measurement at high-demand synchrotrons because the best crystals can be identified in advance, ensuring efficient use of beamtime.
The equipment and the research it will enable are aligned with EPSRC Themes in Physical Sciences, Quantum Technology, Healthcare Technologies and Manufacturing the Future. The proposed equipment will add significant value to EPSRC investment in at least 20 reseach areas across the user base. This will grow over the lifetime of the diffractometer.
The UK is world-leading in analytical science. X-ray crystallography, along with other analytical methods such as NMR spectroscopy, microscopy, and mass spectrometry, are at the heart of the most important research. A major aim of our project is, therefore, to enhance national strategic provision in analytical science in a broader sense.
X-ray crystallography is the most important technique for determining the structures of crystalline solids. The UK boasts a history of pioneering discovery in crystallography, including several Nobel Prizes. Today, the strength of the research base is such that the UK leads the world in crystallography. The reach and impact of the technique is remarkable, spanning chemistry, life sciences, materials science, condensed matter physics and earth sciences, and incorporating a broad community of industrial and academic users.
The vision for our proposal is to enable rapid structure determination across length scales, from small molecules and supramolecules to chemical-biological systems and extended solids. Examples of these materials include catalysts, molecular magnets, pharmaceutical ingredients, polymers, amphiphiles, drug molecules bound to biological targets, energy materials and metal-organic frameworks. Many of these materials form as very small crystals that are difficult or impossible to measure in full on existing in-house diffractometers, which limits the value of the structural information and acts as a barrier to its downstream implementation. We propose to use striking recent advances in diffraction technology, including the availability of X-ray beams with unprecedentedly high brilliance and detectors with very high sensitivity, that will enable the measurement of such crystals. The resulting information will enable the development of more accurate structure-function relationships for the materials of interest.
The automated robotic sample changer will provide game-changing capability. Conventional approaches to single-crystal measurements can be time-consuming, requiring hands-on effort to mount, centre and measure individual crystals. The robot will allow multiple consecutive measurements of single crystals without the need for human intervention. Automation then allows the quality of the crystals to be ranked and the best one selected for further measurements. This will be of immediate benefit to the majority of the user base, whose samples will be measured in full in Sussex. It will also benefit users with samples that require further measurement at high-demand synchrotrons because the best crystals can be identified in advance, ensuring efficient use of beamtime.
The equipment and the research it will enable are aligned with EPSRC Themes in Physical Sciences, Quantum Technology, Healthcare Technologies and Manufacturing the Future. The proposed equipment will add significant value to EPSRC investment in at least 20 reseach areas across the user base. This will grow over the lifetime of the diffractometer.
The UK is world-leading in analytical science. X-ray crystallography, along with other analytical methods such as NMR spectroscopy, microscopy, and mass spectrometry, are at the heart of the most important research. A major aim of our project is, therefore, to enhance national strategic provision in analytical science in a broader sense.
| Description | This award supported the installation of a key item of capital strategic equipment. The instrument has operating well for about a year, but with a few technical issues along the way. The manufacturer has always been very quick to respond. A no-cost extension has been applied to the warranty. The diffractometer is now generating excellent data. |
| Exploitation Route | Given that this is a multiuser item of equipment, we expect the outcomes of this funding to be taken and put to use by many other groups. We have hosted researchers from Bath, Surrey and KCL. |
| Sectors | Chemicals Pharmaceuticals and Medical Biotechnology |
| Title | Data for paper: Single-molecule Magnet Properties of Silole- and Stannole-ligated Erbium Cyclo-octatetraenyl Sandwich Complexes |
| Description | X-ray crystallography data for all compounds in .cif format.check_cif files for all compounds.FTIR data for all compounds.NMR data for stannole.Raw magnetic data in .dat format.AbstractThe synthesis, structures and magnetic properties of an ?5-silole complex and an ?5-stannole complex of erbium are reported. The sandwich complex anions [(?5-CpSi)Er(?8-COT)]- and [(?5-CpSn)Er(?8-COT)]-, where CpSi is [SiC4-2,5-(SiMe3)2-3,4-Ph2]2- (1Si), CpSn is [SnC4-2,5-(SiMe3)2-3,4-Me2]2- (1Sn) and COT = cyclo-octatetraenyl, were obtained as their [K(2.2.2-cryptand)]+ salts and found to be isostructural, with remarkably similar bond lengths and angles, differing only in the lengths of the Er-E interactions (E = Si, Sn). The parallels in the molecular structures of 1Si and 1Sn are reflected in their dynamic magnetic properties, which show single-molecule magnet behaviour in zero applied field, with effective energy barriers of 115 ± 7 and 125 ± 3 cm-1, respectively, along with comparable magnetic relaxation times. Analysis of the two complexes using ab initio calculations reveals differences at a quantitative level, but overall similar electronic structures, with the thermally activated relaxation likely to proceed via the first-excited Kramers doublet. Comparing 1Si and 1Sn with the previously reported germanium analogue 1Ge reveals that swapping one heavier group 14 element for another in complexes of the type [(?5-CpE)Er(?8-COT)]- has a minimal impact on the SMM behaviour. |
| Type Of Material | Database/Collection of data |
| Year Produced | 2025 |
| Provided To Others? | Yes |
| URL | https://sussex.figshare.com/articles/dataset/Data_for_paper_Single-molecule_Magnet_Properties_of_Sil... |