Synthesis of IrIII Hydrido Complexes by Oxidative Addition of Halogenated Theophylline and Adenine Derivatives

ACS Omega
Jonas BlumenbergF Ekkehardt Hahn

Abstract

The IrIII hydrido complexes [1] and [2] have been synthesized by the regioselective oxidative addition of the N7-H bond of 8-halogenotheophyllines to [IrCl(coe)2]2 in the presence of PPh3. The use of dppf in this reaction yielded the bimetallic IrIII/FeII hydrido complexes [3] and [4]. X-ray diffraction studies confirmed that complexes [1]-[4] feature a theophyllinato ligand coordinated to the metal center in the rarely observed, chelating fashion via the N7 and O1 atoms. In addition, 8-bromoadenine reacts with [IrCl(coe)2]2 in the presence of PPh3 to form the IrIII hydrido complex [5] which features one anionic 8-bromoadeninato and one neutral 8-bromoadenine ligand linked by an intramolecular hydrogen bond. Complex [5] was characterized by high-resolution mass spectrometry and an X-ray diffraction analysis but could not be analyzed by nuclear magnetic resonance spectroscopy because of its low solubility.

References

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Jan 29, 2011·Journal of the American Chemical Society·Tim KösterkeF Ekkehardt Hahn
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Jun 26, 2018·Chemical Reviews·Shigeki Kuwata, F Ekkehardt Hahn

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Methods Mentioned

BETA
nuclear magnetic resonance
X-ray
NMR

Software Mentioned

SHELXL
SHELXT

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