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Synthesis of Uranium(VI) Terminal Oxo Complexes: Molecular Geometry Driven by the Inverse Trans-Influence

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† Inorganic Chemistry, Department of Chemistry and Pharmacy, Friedrich-Alexander-University of Erlangen-Nuremberg, Egerlandstrasse 1, 91058 Erlangen, Germany
‡ School of Chemistry, University of Nottingham, University Park, Nottingham NG7 2RD, U.K.
[email protected]
Cite this: J. Am. Chem. Soc. 2012, 134, 11, 5284–5289
Publication Date (Web):February 24, 2012
https://doi.org/10.1021/ja211618v
Copyright © 2012 American Chemical Society
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    Abstract

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    Oxidation of our previously reported uranium(V) oxo complexes, supported by the chelating (RArO)3tacn3– ligand system (R = tert-butyl (t-Bu), 1-t-Bu; R = 1-adamantyl (Ad), 1-Ad), yields terminal uranium(VI) oxo complexes [((RArO)3tacn)U(VI)(O)]SbF6 (R = t-Bu, 2-t-Bu; R = Ad, 2-Ad). These complexes differ in their molecular geometry in that 2-t-Bu possesses pseudo-Cs symmetry in solution and solid state as the terminal oxo ligand lies in the equatorial plane (as defined by the three aryloxide arms of the ligand) in order to accommodate the thermodynamic preference of high-valent uranium oxo complexes to have a σ- and π-donating ligand trans to the oxo (vis-à-vis the ubiquity of the linear UO22+ moiety). The distortion of the ligand — which stands in contrast to all other complexes of uranium supported by the (RArO)3tacn3– ligand, including 2-Ad — is most clearly seen in the structures of 2-t-Bu, [((t-BuArO)3tacn)U(VI)(O)eq]SbF6, and 3-t-Bu, [((t-BuArO)3tacn)U(VI)(O)eq(OC(O)CF3)ax]. The solid-state structure of 3-t-Bu reveals that the trans U–OArO bond length is shortened by 0.1 Å in comparison to the cis U–OArO bonds and the trans U–O–Cipso angle is linearized (157.67° versus 147.85° and 130.03°). Remarkably, the minor modification of the ligand to have Ad groups at the ortho positions of the aryloxide arms is sufficient to stabilize a C3v-symmetric terminal uranium(VI) oxo complex (2-Ad) without a ligand trans to the oxo. These experimental results were reproduced in DFT calculations and allow the qualitative bracketing of the relative thermodynamic stabilization afforded by the inverse trans-influence as ∼6 kcal mol–1.

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    General considerations, UV–vis spectra, crystallographic techniques and tables, electrochemical data, synthetic details for 4-t-Bu, and computational details for 2-t-Bu, 2-Ad, and 3-t-Bu (PDF, CIF). This material is available free of charge via the Internet at http://pubs.acs.org.

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