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. 2022 Sep 28;144(38):17423-17431.
doi: 10.1021/jacs.2c04947. Epub 2022 Sep 19.

Actinide-Oxygen Multiple Bonds from Air: Synthesis and Characterization of a Thorium Oxo Supported by Redox-Active Ligands

D M Ramitha Y P Rupasinghe  1 , Makayla R Baxter  1 , Himanshu Gupta  2 , Andrew T Poore  1 , Robert F Higgins  2 , Matthias Zeller  1 , Shiliang Tian  1 , Eric J Schelter  2 , Suzanne C Bart  1
Affiliations

Actinide-Oxygen Multiple Bonds from Air: Synthesis and Characterization of a Thorium Oxo Supported by Redox-Active Ligands

D M Ramitha Y P Rupasinghe et al. J Am Chem Soc. .

Abstract

The first non-uranyl, f-element oxo complex synthesized from dioxygen in dry air is presented in this work. The synthesis was accomplished by treating the redox-active thorium amidophenolate complex, [Th(dippap)3][K(15-c-5)2]2 (1-ap crown), with dioxygen in dry air, forming a rare terminal thorium oxo, [O═Th(dippisq)2(dippap)][K(15-c-5)2]2 (2-oxo). Compound 1-ap crown was regenerated by treating 2-oxo with potassium graphite. X-ray crystallography of 2-oxo revealed a comparatively longer bond length for the thorium-oxygen double bond when compared to other thorium oxos. As such, several thorium-oxygen single bonds were synthesized for comparison, including Th(dippisq)2(OSiMe3)2(THF) (4-OSiMe3), Th(OSiMe3)4(bipy)2 (5-OSiMe3), and [Th(OH)2 (dippHap)4][K(15-c-5)2]2 (6-OH). Full spectroscopic and structural characterization of the complexes was performed via 1H NMR spectroscopy, X-ray crystallography, EPR spectroscopy, and electronic absorption spectroscopy as well as SQUID magnetometry, which all confirmed the electronic structure of these complexes.

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