MRI: Acquisition of a Single-Crystal Diffractometer for Chemistry and Materials Research

Overview : The aim of this proposal is to acquire a MoKa microsource small-molecule diffractometer to support a broad spectrum of research, education, and outreach activities. The diffractometer will provide accurate and precise structural information, which is essential for rationalizing the structure-property relationships required to design and improve functional materials. The instrument is fundamental to research in fields that require chemical structure data, including chemistry, pharmacy, toxicology, materials science, and condensed matter physics. The diffractometer will form the core of instructional and outreach efforts in small-molecule crystallography at the University of Kentucky (UK) and for students at local colleges and high schools. It will replace an obsolete (1997 vintage) kappaCCD system, which is slow, inefficient, lacks much needed functionality, and is not cost effective to maintain. Capabilities enabled by the micro-focus X-ray source and new-technology CMOS X-ray detector include, but are not limited to: 1) rapid data collection (minutes/hours vs. hours/days); 2) extremely small crystals (>10x smaller than the kappaCCD); 3) time-resolved diffraction; 4) structural studies on in-situ phase transitions and polymorphism; 5) Twinned crystals and other aggregates (the kappaCCD software has only rudimentary twin functionality). Intellectual Merit: The UK X-Ray Facility is a national and international resource, providing essential high-quality structural data to research ranging from the development of materials for organic electronics (e.g., flexible displays and photovoltaics) to the fundamentals of catalysis and reaction mechanisms. Recent work developing improved additives for rechargeable batteries, photodynamic agents for biotechnological applications, natural products with important biological activities, and 'green' reagents for carbon capture in coal-fired power plants is critically dependent on rapid-turnaround, accurate molecular and crystal structure information. The proposed instrument will upgrade and expand the services available to researchers at UK and elsewhere, across a wide range of research disciplines, thereby accelerating the development of improved compounds with applications in materials science, chemistry, catalysis, biotechnology, energy storage, and pollution control. Broader Impacts: This proposal to modernize our research infrastructure will directly benefit many scientists in diverse fields at UK, at nearby institutions, and via collaborations, with institutions across the globe. The diffractometer will complement existing facilities at UK, including the NSF-EPSCoR-funded Center for Advanced Materials (CAM), and will support the research of ten other research groups in Chemistry, and similar numbers in Physics, Pharmacy, Biochemistry, and the Center for Applied Energy Research (CAER). Undergraduate institutions in the region will enjoy no-cost access to the Facility, its instrumentation, and the crystallographic expertise of the PI. The diffractometer will also be used in research collaborations beyond the state of Kentucky (notably, U. Mass., Stanford, and Princeton). Given the increased capabilities of modern equipment, the new diffractometer will not only replace an obsolete system, but will promote dramatically higher productivity. Microsource generators produce X-ray beams of much higher brilliance than conventional sealed-tube sources, and do so at a much lower nominal power load. Combined with the air-cooled CMOS detector, this negates the need for cooling water, bringing concomitant reductions in complexity, and tangible savings in energy usage. Beyond UK, the diffractometer will foster growth of our network of collaborators that rely on the UK X-Ray Facility. Instructional and outreach activities at the graduate, undergraduate, and high-school levels will benefit not only UK personnel, but also students at colleges and high schools in the region. Under the direction of the PI, this new state-of-the-art system will be used for teaching in a laboratory-based crystallography course, for class assignments in our undergraduate inorganic chemistry teaching laboratories, and in ad-hoc training of Faculty, post-docs, students, visiting scholars, summer students, high-school senior interns, and students from UK's high-school STEAM academy. The rapid turnaround will provide students with analysis results within a single class session. Motivated students will be able to perform work on their own (with appropriate guidance). With the help of a soon-to-be-retired Faculty member and world-class crystallographer, Prof. Carol Brock, the instrument will be used in open-house demonstrations and workshops for undergraduates and high-school students, especially those from nearby Appalachia and other areas historically underrepresented in the sciences.