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Solvent responsive catalyst improves NMR sensitivity via efficient magnetisation transfer.

Amy J Ruddlesden1, Simon B Duckett1

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This study introduces a novel iridium carbene complex that acts as a precursor for effective magnetisation transfer catalysts. The catalyst

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Area of Science:

  • Organometallic Chemistry
  • Catalysis
  • Nuclear Magnetic Resonance (NMR) Spectroscopy

Background:

  • Development of novel catalysts for enhanced chemical reactions.
  • Importance of understanding solvent effects on catalyst structure and activity.
  • Magnetisation transfer and parahydrogen-induced polarisation (PHIP) techniques.

Purpose of the Study:

  • Synthesize and characterize a new bidentate iridium carbene complex.
  • Investigate its role as a precursor for magnetisation transfer catalysts.
  • Determine the solvent-dependent nature of the active catalyst species and their performance.

Main Methods:

  • Synthesis of the iridium carbene complex Ir(κC,O-L1)(COD).
  • Catalyst activation via reaction with H2 and a two-electron donor.
  • Analysis of catalyst structure and hydride ligand symmetry in different solvents (benzene/pyridine vs. methanol).
  • Evaluation of catalytic activity using parahydrogen-induced polarisation (PHIP) in (1)H NMR.

Main Results:

  • Formation of neutral and zwitterionic iridium complexes depending on the solvent.
  • Demonstration of solvent-dependent hydride ligand symmetry (inequivalent vs. equivalent).
  • Achieved significant proton polarisation levels (up to ≈1.2%) in target molecules via SABRE (Signal Amplification By Reversible Exchange).

Conclusions:

  • Rational catalyst design leads to solvent-dependent magnetisation transfer catalysts.
  • The study highlights the crucial role of solvent in dictating catalyst form and activity.
  • The developed iridium complex shows promising activity for polarisation transfer using parahydrogen.