A regionally strategic NMR spectrometer with globally unique high pressure and reaction monitoring capability
Lead Research Organisation:
University of Manchester
Department Name: Chemistry
Abstract
Nuclear magnetic resonance (NMR) spectroscopy is one of the most useful methods for studying the structures and behaviours of molecules, and is of critical importance both in understanding the world around us and in developing new technologies. It is a powerful tool for determining the structures of pure compounds, the characteristics and composition of materials, and for monitoring chemical reactions.
Chemists, and materials and life scientists, fight a continual battle to extract qualitative and quantitative information from the increasingly complex fruits of their research. The utility of NMR spectrometers has made them ubiquitous in chemistry departments. However, as more and more complex problems are tackled, extracting the chemical information needed is becoming increasingly difficult with standard NMR instrumentation. Many spectra are either too complex to analyse, with too many overlapped signals, or have signal strengths below the detection limit.
A new high sensitivity, high resolution NMR spectrometer is urgently needed in Manchester to support advances in the physical sciences. The instrument will operate at a 1H frequency of 700 MHz, giving very high resolution, and will be equipped with a liquid helium-cooled probe, giving very high sensitivity and a low limit of detection for liquid samples. It will also have the capability to study a wide range of nuclei in the solid state. The spectrometer will be integratable into a high pressure system that flows chemical reaction mixtures through the instrument, allowing reactant and product concentrations to be measured in real time and providing unique access to information about high pressure reaction behaviour.
The instrument will underpin a broad range of research areas including Catalysis, Chemical Reaction Dynamics and Mechanisms, Synthetic Organic Chemistry, Synthetic Supramolecular Chemistry, Polymer Materials, Energy Storage, Functional Ceramics and Inorganics, Nuclear Fission, Synthetic Coordination Chemistry, Synthetic Biology, and Chemical Biology and Biological Chemistry.
The proposed spectrometer will provide regionally strategic capabilities - high sensitivity and high resolution, optimised for chemical applications - and underpin and complement EPSRC facilities and high field NMR instrumentation nationally.
Chemists, and materials and life scientists, fight a continual battle to extract qualitative and quantitative information from the increasingly complex fruits of their research. The utility of NMR spectrometers has made them ubiquitous in chemistry departments. However, as more and more complex problems are tackled, extracting the chemical information needed is becoming increasingly difficult with standard NMR instrumentation. Many spectra are either too complex to analyse, with too many overlapped signals, or have signal strengths below the detection limit.
A new high sensitivity, high resolution NMR spectrometer is urgently needed in Manchester to support advances in the physical sciences. The instrument will operate at a 1H frequency of 700 MHz, giving very high resolution, and will be equipped with a liquid helium-cooled probe, giving very high sensitivity and a low limit of detection for liquid samples. It will also have the capability to study a wide range of nuclei in the solid state. The spectrometer will be integratable into a high pressure system that flows chemical reaction mixtures through the instrument, allowing reactant and product concentrations to be measured in real time and providing unique access to information about high pressure reaction behaviour.
The instrument will underpin a broad range of research areas including Catalysis, Chemical Reaction Dynamics and Mechanisms, Synthetic Organic Chemistry, Synthetic Supramolecular Chemistry, Polymer Materials, Energy Storage, Functional Ceramics and Inorganics, Nuclear Fission, Synthetic Coordination Chemistry, Synthetic Biology, and Chemical Biology and Biological Chemistry.
The proposed spectrometer will provide regionally strategic capabilities - high sensitivity and high resolution, optimised for chemical applications - and underpin and complement EPSRC facilities and high field NMR instrumentation nationally.
Publications
Hutchinson G
(2021)
Mechanistically Guided Design of an Efficient and Enantioselective Aminocatalytic a-Chlorination of Aldehydes.
in Journal of the American Chemical Society
Taylor DA
(2021)
SABRE-enhanced real-time pure shift NMR spectroscopy.
in Magnetic resonance in chemistry : MRC
Du J
(2021)
Exceptional uranium(VI)-nitride triple bond covalency from 15N nuclear magnetic resonance spectroscopy and quantum chemical analysis.
in Nature communications
Alamillo-Ferrer C
(2021)
Understanding the Diastereopreference of Intermediates in Aminocatalysis: Application to the Chiral Resolution of Lactols.
in The Journal of organic chemistry
Ma Y
(2022)
Direct Observation of Ammonia Storage in UiO-66 Incorporating Cu(II) Binding Sites.
in Journal of the American Chemical Society
Smith MJ
(2022)
Giving Pure Shift NMR Spectroscopy a REST-Ultrahigh-Resolution Mixture Analysis.
in Analytical chemistry
Seed JA
(2022)
A Series of Rare-Earth Mesoionic Carbene Complexes.
in Chemistry (Weinheim an der Bergstrasse, Germany)
Dumon AS
(2022)
A computational tool to accurately and quickly predict 19F NMR chemical shifts of molecules with fluorine-carbon and fluorine-boron bonds.
in Physical chemistry chemical physics : PCCP
Seed JA
(2022)
Mesoionic Carbene Complexes of Uranium(IV) and Thorium(IV).
in Organometallics
Di Carmine G
(2023)
Humin Formation on SBA-15-pr-SO 3 H Catalysts during the Alcoholysis of Furfuryl Alcohol to Ethyl Levulinate: Effect of Pore Size on Catalyst Stability, Transport, and Adsorption
in ACS Applied Materials & Interfaces
Caytan E
(2023)
Recovering sensitivity lost through convection in pure shift NMR.
in Chemical communications (Cambridge, England)
Huang W
(2023)
Direct Synthesis of N-formamides by Integrating Reductive Amination of Ketones and Aldehydes with CO 2 Fixation in a Metal-Organic Framework
in Chemistry - A European Journal
Du J
(2023)
31P Nuclear Magnetic Resonance Spectroscopy as a Probe of Thorium-Phosphorus Bond Covalency: Correlating Phosphorus Chemical Shift to Metal-Phosphorus Bond Order.
in Journal of the American Chemical Society
Gates E
(2023)
Solvent suppression in pure shift NMR
Alamillo-Ferrer C
(2023)
Mechanistic interpretation of orders in catalyst greater than one.
in Nature reviews. Chemistry
Yang X
(2023)
Bismuth-Catalyzed Amide Reduction.
in Angewandte Chemie (International ed. in English)
Grose LA
(2023)
Olefin hydroboration catalyzed by an iron-borane complex.
in Chemical communications (Cambridge, England)
Gates EL
(2023)
Ultra-selective, ultra-clean 1D rotating-frame Overhauser effect spectroscopy.
in Chemical communications (Cambridge, England)
Burés J
(2023)
Organic reaction mechanism classification using machine learning.
in Nature
Taylor DA
(2023)
Ultra-selective 1D clean in-phase correlation spectroscopy.
in Chemical communications (Cambridge, England)
Deakin C
(2024)
Rare earth mixed sandwich complexes with tetraalkylphospholide and cyclooctatetraenide ligands
in Journal of Organometallic Chemistry
Bennett TS
(2024)
Studying Cation Exchange in {Cr7Co} Pseudorotaxanes: Preparatory Studies for Making Hybrid Molecular Machines.
in Chemistry (Weinheim an der Bergstrasse, Germany)
| Description | The UK Dynamic Nuclear Polarisation Magic Angle Spinning NMR Facility |
| Amount | £2,867,300 (GBP) |
| Funding ID | EP/W021463/1 |
| Organisation | Engineering and Physical Sciences Research Council (EPSRC) |
| Sector | Public |
| Country | United Kingdom |
| Start | 04/2022 |
| End | 04/2027 |
| Title | Acetone NMR data |
| Description | Raw, unprocessed NMR spectra obtained in d-acetone |
| Type Of Material | Database/Collection of data |
| Year Produced | 2023 |
| Provided To Others? | Yes |
| Impact | Dataset supporting research article. Allows results to be more easily reproduced by other researchers. |
| URL | https://figshare.manchester.ac.uk/articles/dataset/Acetone_NMR_data/24771504 |
| Title | Convection-compensated pure shift NMR |
| Description | This archive contains all raw experimental data files, macros, pulse sequence code, shaped pulse definitions and Mathematica notebooks to support the article "Convection-compensated pure shift NMR: how to stop convection ruining experiments." |
| Type Of Material | Database/Collection of data |
| Year Produced | 2023 |
| Provided To Others? | Yes |
| Impact | Dataset supporting research article. Allows results to be more easily reproduced by other researchers. |
| URL | https://figshare.manchester.ac.uk/articles/dataset/Convection-compensated_pure_shift_NMR/23864202 |
| Title | Kinetic NMR spectra 700MHz |
| Description | Raw NMR files for Kinetic studies of thread exchange |
| Type Of Material | Database/Collection of data |
| Year Produced | 2023 |
| Provided To Others? | Yes |
| Impact | Dataset supporting research article. Allows results to be more easily reproduced by other researchers. |
| URL | https://figshare.manchester.ac.uk/articles/dataset/Kinetic_NMR_spectra_700MHz/24771522 |
| Title | Parameter estimation simulation data COPASI |
| Description | Parameter estimation results COPASI 1-10 |
| Type Of Material | Database/Collection of data |
| Year Produced | 2023 |
| Provided To Others? | Yes |
| Impact | Dataset supporting research article. Allows results to be more easily reproduced by other researchers. |
| URL | https://figshare.manchester.ac.uk/articles/dataset/Parameter_estimation_simulation_data_COPASI/24771... |
| Title | Pure Shift 2D NMR Spectroscopy |
| Description | raw experimental data for the book chapter "Pure Shift 2D NMR Spectroscopy" |
| Type Of Material | Database/Collection of data |
| Year Produced | 2022 |
| Provided To Others? | Yes |
| Impact | Dataset supporting book chapter. Allows results to be more easily reproduced by other researchers. |
| URL | https://figshare.manchester.ac.uk/articles/dataset/Pure_Shift_2D_NMR_Spectroscopy/19729807 |
| Title | Solvent suppression in pure shift NMR |
| Description | This folder contains all NMR raw data for the publication entitled "Solvent suppression in pure shift NMR", as well as relevant pulse programs for Bruker spectrometers. Detailed description of the folder contain can be found in the read-me file. |
| Type Of Material | Database/Collection of data |
| Year Produced | 2023 |
| Provided To Others? | Yes |
| Impact | Dataset supporting research article. Allows results to be more easily reproduced by other researchers. |
| URL | https://figshare.manchester.ac.uk/articles/dataset/Solvent_suppression_in_pure_shift_NMR/24600114 |
| Title | T1 Relaxation data NMR |
| Description | T1 Paramagnetic NMR raw data |
| Type Of Material | Database/Collection of data |
| Year Produced | 2023 |
| Provided To Others? | Yes |
| Impact | Dataset supporting research article. Allows results to be more easily reproduced by other researchers. |
| URL | https://figshare.manchester.ac.uk/articles/dataset/T1_Relaxation_data_NMR/24771678 |