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
Iuga D
(2011)
Double-quantum homonuclear correlations of spin I=5/2 nuclei.
in Journal of magnetic resonance (San Diego, Calif. : 1997)
Miah HK
(2013)
Measuring proton shift tensors with ultrafast MAS NMR.
in Journal of magnetic resonance (San Diego, Calif. : 1997)
Martin R
(2012)
An examination of the calcium and strontium site distribution in bioactive glasses through isomorphic neutron diffraction, X-ray diffraction, EXAFS and multinuclear solid state NMR
in Journal of Materials Chemistry
Li A
(2011)
Insights into new calcium phosphosilicate xerogels using an advanced characterization methodology
in Journal of Non-Crystalline Solids
Grigg A
(2015)
Vitrification of ß-tricalcium phosphate in sodium aluminoborophosphate glass and the effect of Ga3+ substitution
in Journal of Solid State Chemistry
Grigg A
(2014)
Cation substitution in ß-tricalcium phosphate investigated using multi-nuclear, solid-state NMR
in Journal of Solid State Chemistry
Webber AL
(2011)
Identifying guanosine self assembly at natural isotopic abundance by high-resolution 1H and 13C solid-state NMR spectroscopy.
in Journal of the American Chemical Society
Stewart KL
(2016)
Atomic Details of the Interactions of Glycosaminoglycans with Amyloid-ß Fibrils.
in Journal of the American Chemical Society
Blanc F
(2011)
Defects in doped LaGaO3 anionic conductors: linking NMR spectral features, local environments, and defect thermodynamics.
in Journal of the American Chemical Society
Bonhomme C
(2012)
87Sr solid-state NMR as a structurally sensitive tool for the investigation of materials: antiosteoporotic pharmaceuticals and bioactive glasses.
in Journal of the American Chemical Society
Sanz Camacho P
(2015)
Unusual intermolecular "through-space" j couplings in p-se heterocycles.
in Journal of the American Chemical Society
Kim G
(2015)
Characterization of the dynamics in the protonic conductor CsH2PO4 by ¹7O solid-state NMR spectroscopy and first-principles calculations: correlating phosphate and protonic motion.
in Journal of the American Chemical Society
Buannic L
(2012)
Probing cation and vacancy ordering in the dry and hydrated yttrium-substituted BaSnO3 perovskite by NMR spectroscopy and first principles calculations: implications for proton mobility.
in Journal of the American Chemical Society
Lamley JM
(2014)
Solid-state NMR of a protein in a precipitated complex with a full-length antibody.
in Journal of the American Chemical Society
Peters GM
(2014)
A G4·K? hydrogel stabilized by an anion.
in Journal of the American Chemical Society
Tatton AS
(2013)
Probing hydrogen bonding in cocrystals and amorphous dispersions using (14)N-(1)H HMQC solid-state NMR.
in Molecular pharmaceutics
Krachmalnicoff A
(2016)
The dipolar endofullerene HF@C60.
in Nature chemistry
Simmons TJ
(2016)
Folding of xylan onto cellulose fibrils in plant cell walls revealed by solid-state NMR.
in Nature communications
Zhang Y
(2016)
Golgi-localized STELLO proteins regulate the assembly and trafficking of cellulose synthase complexes in Arabidopsis.
in Nature communications
Howes AP
(2011)
Boron environments in Pyrex® glass--a high resolution, Double-Rotation NMR and thermodynamic modelling study.
in Physical chemistry chemical physics : PCCP
Haies IM
(2015)
(14)N overtone NMR under MAS: signal enhancement using symmetry-based sequences and novel simulation strategies.
in Physical chemistry chemical physics : PCCP
Baxter EF
(2015)
Combined experimental and computational NMR study of crystalline and amorphous zeolitic imidazolate frameworks.
in Physical chemistry chemical physics : PCCP
Lamley JM
(2015)
Unraveling the complexity of protein backbone dynamics with combined (13)C and (15)N solid-state NMR relaxation measurements.
in Physical chemistry chemical physics : PCCP
Alderman OL
(2013)
Spectral assignments and NMR parameter-structure relationships in borates using high-resolution 11B NMR and density functional theory.
in Physical chemistry chemical physics : PCCP
Johnston KE
(2011)
93Nb NMR and DFT investigation of the polymorphs of NaNbO3.
in Physical chemistry chemical physics : PCCP
Dawson DM
(2013)
High-resolution solid-state 13C NMR spectroscopy of the paramagnetic metal-organic frameworks, STAM-1 and HKUST-1.
in Physical chemistry chemical physics : PCCP
Oliver Alderman (Author)
(2012)
Double Rotation 11B NMR Applied to Polycrystalline Barium Borates
in Physics and Chemistry of Glasses
Davies E
(2014)
Citrate bridges between mineral platelets in bone.
in Proceedings of the National Academy of Sciences of the United States of America
Davies HA
(2014)
Expression and purification of the aortic amyloid polypeptide medin.
in Protein expression and purification
Griffin JM
(2011)
Observation of "hidden" magnesium: first-principles calculations and 25Mg solid-state NMR of enstatite.
in Solid state nuclear magnetic resonance
Reddy GN
(2015)
An NMR crystallography study of the hemihydrate of 2', 3'-O-isopropylidineguanosine.
in Solid state nuclear magnetic resonance
Harris KD
(2015)
Monitoring the evolution of crystallization processes by in-situ solid-state NMR spectroscopy.
in Solid state nuclear magnetic resonance
Blanc F
(2012)
Thermal phase transformations in LaGaO(3) and LaAlO(3) perovskites: an experimental and computational solid-state NMR study.
in Solid state nuclear magnetic resonance
Brown S
(2012)
Applications of high-resolution 1H solid-state NMR
in Solid State Nuclear Magnetic Resonance
Davies HA
(2015)
Comparisons with amyloid-ß reveal an aspartate residue that stabilizes fibrils of the aortic amyloid peptide medin.
in The Journal of biological chemistry
Varghese S
(2016)
High-Resolution Structural Characterization of a Heterogeneous Biocatalyst Using Solid-State NMR
in The Journal of Physical Chemistry C
Fauré N
(2013)
A Solid-State NMR Study of the Immobilization of a-Chymotrypsin on Mesoporous Silica
in The Journal of Physical Chemistry C
Amri M
(2012)
A Multinuclear Solid-State NMR Study of Templated and Calcined Chabazite-Type GaPO-34
in The Journal of Physical Chemistry C
Playford H
(2014)
Characterization of Structural Disorder in ?-Ga 2 O 3
in The Journal of Physical Chemistry C
Mitchell M
(2012)
Exploiting the Chemical Shielding Anisotropy to Probe Structure and Disorder in Ceramics: 89 Y MAS NMR and First-Principles Calculations
in The Journal of Physical Chemistry C
Williams P
(2013)
Expanding the Solid-State Landscape of l -Phenylalanine: Discovery of Polymorphism and New Hydrate Phases, with Rationalization of Hydration/Dehydration Processes
in The Journal of Physical Chemistry C
Hughes CE
(2012)
Exploiting In Situ Solid-State NMR for the Discovery of New Polymorphs during Crystallization Processes.
in The journal of physical chemistry letters
Aliev AE
(2011)
High-resolution solid-state 2H NMR spectroscopy of polymorphs of glycine.
in The journal of physical chemistry. A
Aliev AE
(2013)
Concise NMR approach for molecular dynamics characterizations in organic solids.
in The journal of physical chemistry. A
Aliev AE
(2011)
Natural-abundance solid-state 2H NMR spectroscopy at high magnetic field.
in The journal of physical chemistry. A
Dudenko DV
(2013)
Exploiting the Synergy of Powder X-ray Diffraction and Solid-State NMR Spectroscopy in Structure Determination of Organic Molecular Solids.
in The journal of physical chemistry. C, Nanomaterials and interfaces
Leskes M
(2013)
Monitoring the Electrochemical Processes in the Lithium-Air Battery by Solid State NMR Spectroscopy.
in The journal of physical chemistry. C, Nanomaterials and interfaces
Kenneth Harris (Author)
(2012)
New Strategies for Exploring Crystallization Processes of Organic Materials
in www.amercrystalassn.org
Tatton A
(2012)
14 N- 1 H Heteronuclear Multiple-Quantum Correlation Magic-Angle Spinning NMR Spectroscopy of Organic Solids
in Zeitschrift für Physikalische Chemie
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 |