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Investigation of the Electronic Ground States for a Reduced Pyridine(diimine) Uranium Series: Evidence for a Ligand Tetraanion Stabilized by a Uranium Dimer

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    Investigation of the Electronic Ground States for a Reduced Pyridine(diimine) Uranium Series: Evidence for a Ligand Tetraanion Stabilized by a Uranium Dimer
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    † H.C. Brown Laboratory, Department of Chemistry, Purdue University, West Lafayette, Indiana 47907, United States
    ‡ Department of Chemistry, Supercomputing Institute, and Chemical Theory Center, University of Minnesota, Minneapolis, Minnesota 55455, United States
    § P. Roy and Diana T. Vagelos Laboratories, Department of Chemistry, University of Pennsylvania, Philadelphia, Pennsylvania 19104, United States
    ∥ Los Alamos National Laboratory, Los Alamos, New Mexico 87545, United States
    ⊥ School of Earth Sciences, Environmental Earth System Science Department, Stanford University, Stanford, California 94305-4216, United States
    *[email protected]
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    Cite this: J. Am. Chem. Soc. 2015, 137, 14, 4690–4700
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    https://doi.org/10.1021/ja511867a
    Published April 1, 2015
    Copyright © 2015 American Chemical Society
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    The electronic structures of a series of highly reduced uranium complexes bearing the redox-active pyridine(diimine) ligand, MesPDIMe (MesPDIMe = 2,6-(2,4,6-Me3-C6H2-N═CMe)2C5H3N) have been investigated. The complexes, (MesPDIMe)UI3(THF) (1), (MesPDIMe)UI2(THF)2 (2), [(MesPDIMe)UI]2 (3), and [(MesPDIMe)U(THF)]2 (4), were examined using electronic and X-ray absorption spectroscopies, magnetometry, and computational analyses. Taken together, these studies suggest that all members of the series contain uranium(IV) centers with 5f 2 configurations and reduced ligand frameworks, specifically [MesPDIMe]•/–, [MesPDIMe]2–, [MesPDIMe]3– and [MesPDIMe]4–, respectively. In the cases of 2, 3, and 4 no unpaired spin density was found on the ligands, indicating a singlet diradical ligand in monomeric 2 and ligand electron spin-pairing through dimerization in 3 and 4. Interaction energies, representing enthalpies of dimerization, of −116.0 and −144.4 kcal mol–1 were calculated using DFT for the monomers of 3 and 4, respectively, showing there is a large stabilization gained by dimerization through uranium–arene bonds. Highlighted in these studies is compound 4, bearing a previously unobserved pyridine(diimine) tetraanion, that was uniquely stabilized by backbonding between uranium cations and the η5-pyridyl ring.

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    Cite this: J. Am. Chem. Soc. 2015, 137, 14, 4690–4700
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    https://doi.org/10.1021/ja511867a
    Published April 1, 2015
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