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Issue 6, 2015
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Stabilization of MIV = Ti, Zr, Hf, Ce, and Th using a selenium bis(phenolate) ligand

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Abstract

We report M(IV) M = Ti, Zr, Hf, Ce, and Th, complexes of a selenium bis(phenolate) ligand, 2,2′-selenobis(4,6-di-tert-butylphenol), (H2ArOSeO), 1. Reaction of Ti(NEt2)4 with two equivalents of 1 affords Ti(ArOSeO)2, 2. Salt metathesis of ZrCl4 and HfCl4 with two equivalents of Na2ArOSeO produces Zr(ArOSeO)2(THF), 3, and Hf(ArOSeO)2(THF), 4, respectively. Protonolysis of ThCl[N(SiMe3)2]3 with two equivalents of 1 yields Th(ArOSeO)2(THF)2, 5. Salt metathesis of Ce(OTf)3 and two equivalents of Na2ArOSeO produces [Na(THF)3][Ce(ArOSeO)2], which was oxidized in situ using 0.5 equivalents of I2 to yield the diamagnetic Ce(IV) product, Ce(ArOSeO)2(THF)2, 6. Addition of 2,2′-bipyridyl to 6 forms Ce(ArOSeO)2(bipy), 6a. Each diamagnetic complex was characterized using 1H, 13C, and 77Se NMR and IR spectroscopy and the structures of 2–6a were established with X-ray crystallography. Electrochemical measurements using cyclic voltammetry on complexes 2, 5, and 6 are also reported.

Graphical abstract: Stabilization of MIV = Ti, Zr, Hf, Ce, and Th using a selenium bis(phenolate) ligand

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Publication details

The article was received on 16 Jun 2014, accepted on 22 Aug 2014 and first published on 11 Sep 2014


Article type: Paper
DOI: 10.1039/C4DT01798F
Citation: Dalton Trans., 2015,44, 2693-2702
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    Stabilization of MIV = Ti, Zr, Hf, Ce, and Th using a selenium bis(phenolate) ligand

    A. C. Behrle, J. R. Levin, J. E. Kim, J. M. Drewett, C. L. Barnes, E. J. Schelter and J. R. Walensky, Dalton Trans., 2015, 44, 2693
    DOI: 10.1039/C4DT01798F

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