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

Dalton Transactions : an International Journal of Inorganic Chemistry
Andrew C BehrleJustin R Walensky

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), (H(2)(Ar)OSeO), 1. Reaction of Ti(NEt(2))(4) with two equivalents of affords Ti((Ar)OSeO)(2), 2. Salt metathesis of ZrCl(4) and HfCl(4) with two equivalents of Na(2)(Ar)OSeO produces Zr((Ar)OSeO)(2)(THF), 3, and Hf((Ar)OSeO)(2)(THF), 4, respectively. Protonolysis of ThCl[N(SiMe(3))(2)](3) with two equivalents of yields Th((Ar)OSeO)(2)(THF)(2), 5. Salt metathesis of Ce(OTf)(3) and two equivalents of Na(2)(Ar)OSeO produces [Na(THF)(3)][Ce((Ar)OSeO)(2)], which was oxidized in situ using 0.5 equivalents of I(2) to yield the diamagnetic Ce(iv) product, Ce((Ar)OSeO)(2)(THF)(2), 6. Addition of 2,2'-bipyridyl to forms Ce((Ar)OSeO)(2)(bipy), 6a. Each diamagnetic complex was characterized using (1)H, (13)C, and (77)Se 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 6a re also reported.

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Citations

Oct 16, 2015·Dalton Transactions : an International Journal of Inorganic Chemistry·Qiu SunQi Shen
Jul 4, 2017·Inorganic Chemistry·Jochen FriedrichReiner Anwander
Jul 13, 2018·Dalton Transactions : an International Journal of Inorganic Chemistry·Jochen FriedrichReiner Anwander
Sep 1, 2018·Chemical Communications : Chem Comm·Alexander J MyersJustin R Walensky
May 8, 2018·Chemical Science·Nicholas S Settineri, John Arnold
Sep 24, 2020·Chemistry : a European Journal·Moya A Hay, Colette Boskovic
May 24, 2019·Journal of the American Chemical Society·Thibault CheissonEric J Schelter
Oct 9, 2020·Inorganic Chemistry·Roger KloditzJuliane März
Aug 24, 2017·Inorganic Chemistry·Matthew A StuberJohn G Brennan
Feb 5, 2019·Journal of the American Chemical Society·Shane S GalleySuzanne C Bart

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