Solid-State NMR at 850 MHz: A World-leading UK Facility to deliver Advances in Materials Science, Chemistry, Biology, Earth Science and Physics

Lead Research Organisation: University of Warwick
Department Name: Physics

Abstract

It is the structural arrangement and motion of molecules and ions that determine, e.g., the bulk properties of a material or the function of biomolecules. Therefore, the availability of state-of-the-art analytical infrastructure for probing atomic-level structure and dynamics is essential to enable advances across science. The power of solid-state Nuclear Magnetic Resonance (NMR) as such a probe is being increasingly demonstrated by applications to, e.g., materials for hydrogen storage and radioactive waste encapsulation, pharmaceutical formulations, and the amyloid plaques associated with diseases such as Alzheimer's. Solid-state NMR is most sensitive to the local chemical structure (usually up to a few bond lengths) around a particular nucleus and is thus well suited to characterising the many important systems that lack periodic order, making it complementary to well-established diffraction techniques.To extend the applicability of NMR, two key limiting factors must be addressed: sensitivity, i.e., the relative intensity of spectral peaks as compared to the noise level, and resolution, i.e., the linewidths of individual peaks that determine whether two close-together signals can be separately observed. Both sensitivity and resolution are much improved by performing NMR experiments at higher magnetic field, thus making possible applications that are not feasible at lower field. Hence, this proposal is to establish a UK facility for solid-state NMR at a world-leading magnetic field strength of 20 Tesla, corresponding to a frequency for the 1H hydrogen nucleus of 850 MHz. The resonant frequency of different nuclear isotopes are well separated such that an NMR spectrum is specific to a particular chosen isotope. NMR experiments at 20 Tesla will make use of as much of the Periodic Table as possible. A particular focus will be on nuclei which are difficult due to their low natural abundance or low resonance frequency - there are many important so-called low-gamma nuclei, e.g., 25Mg, 33S, 39K, 43Ca, 47/49Ti, with resonance frequencies < 10% of 1H. High magnetic field is especially important for the study of the over two thirds of NMR-active isotopes (i.e., with non-zero spin) that possess a quadrupolar electric moment, i.e., a non-spherical distribution of electric charge. For nuclei with spin 1/2, e.g., 13C, the routinely applied technique of physically rotating the sample around an axis inclined at the so-called magic angle of 54.7 degrees to the magnetic field direction yields narrow resonance peaks. However, for the many quadrupolar nuclei with half-integer spin, a residual broadening remains in the magic-angle spinning experiment. This residual quadrupolar broadening (in the usual NMR scale of ppm) is inversely proportional to the magnetic field squared; as well as improving resolution, the concentration of the signal intensity into a narrower lineshape hence means a still greater sensitivity dependence on the magnetic field strength. Oxygen is a key constituent of most organic and inorganic compounds; however, it is difficult to study by NMR since the only NMR-active isotope is the quadrupolar nucleus 17O, whose natural abundance is only 0.037 %. Nearly all NMR studies to date have required the preparation of 17O-labelled samples (starting with 17O-enriched water); very excitingly, working at 20 Tesla offers the possibility of recording high-resolution 17O spectra at natural abundance.A test of a powerful technique is its applicability to a wide range of problems. The high-field solid-state NMR facility will make possible experiments that provide unique information for applications across science, ranging from materials for catalysis, radioactive waste encapsulation, dental implants, batteries, drug delivery, through gaining new understanding of geological processes, to the life sciences, e.g., amyloid plaques, metal-binding proteins, bone structure, membrane proteins, enzymes.

Publications

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Aliev AE (2013) Concise NMR approach for molecular dynamics characterizations in organic solids. in The journal of physical chemistry. A

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Aliev AE (2011) High-resolution solid-state 2H NMR spectroscopy of polymorphs of glycine. in The journal of physical chemistry. A

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Aliev AE (2011) Natural-abundance solid-state 2H NMR spectroscopy at high magnetic field. in The journal of physical chemistry. A

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Antzutkin ON (2012) Hydrogen bonding in Alzheimer's amyloid-ß fibrils probed by 15N{17O} REAPDOR solid-state NMR spectroscopy. in Angewandte Chemie (International ed. in English)

 
Description The grant established the UK 850 MHz Solid-State NMR Facility (now an EPSRC National Research Facility): operational since 2010, this is based around a wide-bore 20 T (or 850 MHz) NMR spectrometer, together with a range of specialised probes, supported by a dedicated Facility Manager and overseen by a Facility Executive and Oversight Committee. Up to the end of this initial grant in 2015, the Facility had been used by 47 distinct PIs from 22 different UK institutions.

Access by the UK scientific community to the 850 MHz Solid-State NMR Facility has provided new insight for a wide range of application areas of economic and social importance:
(i) chemistry, e.g., pharmaceuticals, self-assembled nanostructures, crystallisation phenomena
(ii) materials science, e.g., batteries, catalysts, hydrogen storage and motion, metal-organic frameworks, carbon capture, cement, tissue scaffolds, storage of nuclear waste
(iii) biology, e.g., plant cell walls, protein complexes, membrane proteins, bone and biomineral structure

Industry has accessed the state-of-the-art solid-state NMR instrumentation either via either via paid-for industrial contract research or through industry support of PhD student users of the Facility, for example, the pharmaceutical (e.g., AstraZeneca and GlaxoSmithKline), oil/ fuel (e.g., Infineum and Sasol) and catalysis/ materials (e.g., BP, Johnson Matthey) industry.

The Facility also provides the opportunity for users to share implemented NMR pulse sequences for the benefit of the wider community.
Exploitation Route As examples, specific case studies have been prepared for:
1. NMR Crystallography in Pharmaceutical Development
2. Molecular architecture of plant cell walls
3. NMR spectroscopy of microporous materials
4. Large protein complexes by fast MAS NMR
https://warwick.ac.uk/fac/sci/physics/research/condensedmatt/nmr/850/case_studies/
Sectors Agriculture, Food and Drink,Chemicals,Energy,Healthcare,Manufacturing, including Industrial Biotechology,Pharmaceuticals and Medical Biotechnology

URL https://warwick.ac.uk/fac/sci/physics/research/condensedmatt/nmr/850/annual_reports/
 
Description Access by the UK scientific community to the 850 MHz Solid-State NMR Facility has provided new insight for a wide range of application areas of economic and social importance: (i) chemistry, e.g., pharmaceuticals, self-assembled nanostructures, crystallisation phenomena (ii) materials science, e.g., batteries, catalysts, hydrogen storage and motion, metal-organic frameworks, carbon capture, cement, tissue scaffolds, storage of nuclear waste (iii) biology, e.g., plant cell walls, protein complexes, membrane proteins, bone and biomineral structure Considering specific examples: understanding of intermolecular interactions will lead to better pharmaceutical formulations for enhanced drug delivery; knowledge of the underlying chemistry will enable better energy materials and catalysts to be produced; insight into the molecular basis of plant cell wall properties impacts on recalcitrance, which hinders the use of plant biomass for renewable energy by inhibiting the conversion into fermentable sugars. Industry has accessed the state-of-the-art solid-state NMR instrumentation either via either via paid-for industrial contract research or through industry support of PhD student users of the Facility, for example, the pharmaceutical (e.g., AstraZeneca and GlaxoSmithKline), oil/ fuel (e.g., Infineum and Sasol) and catalysis/ materials (e.g., BP, Johnson Matthey) industry.
First Year Of Impact 2011
Sector Agriculture, Food and Drink,Chemicals,Energy,Healthcare,Manufacturing, including Industrial Biotechology,Pharmaceuticals and Medical Biotechnology
Impact Types Societal,Economic