Journal
CHEMPHYSCHEM
Volume 20, Issue 2, Pages 241-245Publisher
WILEY-V C H VERLAG GMBH
DOI: 10.1002/cphc.201800829
Keywords
carbonates; hyperpolarization; iridium; para-hydrogen; singlet states
Funding
- Wellcome Trust [092506, 098335]
- University of York
- ESPRC
- EPSRC [1941550] Funding Source: UKRI
- MRC [MR/M008991/1] Funding Source: UKRI
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The formation and hyperpolarization of an [Ir(H)(2)(amine)(IMes)(eta(2)-imine)]Cl complex that can be created in a hyperpolarized nuclear singlet state is reported. These complexes are formed when an equilibrium mixture of pyruvate, amine (benzylamine or phenylethylamine), and the corresponding imine condensation product, react with preformed [Ir(H)(2)(amine)(3)(IMes)]Cl. These iridium alpha-carboxyimine complexes exist as two regioisomers differentiated by the position of amine. When examined with para-hydrogen the hydride resonances of the isomer with amine trans to hydride become strongly hyperpolarized. The initial hydride singlet states readily transfer to the corresponding C-13(2) state in the labelled imine and exhibit magnetic state lifetimes of up to 11 seconds. Their C-13 signals have been detected with up to 420 fold signal gains at 9.4 T. On a longer timescale, and in the absence of H-2, further reaction leads to the formation of neutral carbonate containing [Ir(amine)(eta(2)-CO3)(IMes)(eta(2)-imine)]. Complexes are characterized by, IR, MS, NMR and X-ray diffraction.
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