Preprints
https://doi.org/10.5194/mr-2021-23
https://doi.org/10.5194/mr-2021-23

  24 Mar 2021

24 Mar 2021

Review status: this preprint is currently under review for the journal MR.

Determination of hydrogen exchange and relaxation parameters in PHIP complexes at micromolar concentrations

Lisanne Sellies, Ruud L. E. G. Aspers, and Marco Tessari Lisanne Sellies et al.
  • Institute for Molecules and Materials, Radboud University, Nijmegen, 6525AJ, the Netherlands

Abstract. Non-hydrogenative Para-Hydrogen Induced Polarization (PHIP) is a fast, efficient and relatively inexpensive approach to enhance Nuclear Magnetic Resonance (NMR) signals of small molecules in solution. The efficiency of this technique depends on the interplay of NMR relaxation and kinetic processes, which, at high concentrations, can be characterized by selective inversion experiments. However, in the case of dilute solutions this approach is clearly not viable. Here, we present alternative PHIP-based NMR experiments to determine hydrogen and hydrides’ relaxation parameters as well as the rate constants for p-H2 association and dissociation from asymmetric PHIP complexes at micromolar concentrations. Access to these parameters is necessary to understand and improve the PHIP enhancements of (dilute) substrates present in, for instance, biofluids and natural extracts.

Lisanne Sellies et al.

Status: open (until 01 May 2021)

Comment types: AC – author | RC – referee | CC – community | EC – editor | CEC – chief editor | : Report abuse
  • RC1: 'Comment on mr-2021-23', Malcolm Levitt, 09 Apr 2021 reply

Lisanne Sellies et al.

Lisanne Sellies et al.

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Short summary
Reversible para-hydrogen induced polarization (PHIP) is a technique to enhance NMR signals in solution, based on the association/dissociation of para-hydrogen and substrate molecules to an iridium catalyst. In this work we present an approach to measure NMR relaxation as well as rate constants of para-hydrogen association/dissociation to the iridium catalyst. These rates are important to understand the different PHIP efficiency observed for different substrate molecules.