Rigid NON- and NSN-ligand complexes of tetravalent and trivalent uranium: comparison of U-OAr2 and U-SAr2 bonding

Dalton Transactions : an International Journal of Inorganic Chemistry
Balamurugan VidjayacoumarJames F Britten

Abstract

A rigid NSN-donor proligand, 4,5-bis(2,6-diisopropylanilino)-2,7-di-tert-butyl-9,9-dimethylthioxanthene (H(2)[TXA(2)], 1) was prepared by palladium-catalyzed coupling of 2,6-diisopropylaniline with 4,5-dibromo-2,7-di-tert-butyl-9,9-dimethylthioxanthene. Deprotonation of 1 using (n)BuLi provided Li(2)(DME)(2)[TXA(2)] (2), and subsequent reaction with UCl(4) afforded [Li(DME)(3)][(TXA(2))UCl(3)] (4). The analogous NON-donor ligated complex [(XA(2))UCl(3)K(DME)(3)] [3; XA(2) = 4,5-bis(2,6-diisopropylanilino)-2,7-di-tert-butyl-9,9-dimethylxanthene] was prepared by the reaction of K(2)(DME)(x)[XA(2)] with UCl(4). A cyclic voltammogram (CV) of 3 in THF/[NBu(4)][B(C(6)F(5))(4)] at 200 mV s(-1) showed an irreversible reduction to uranium(III) at E(pc) = -2.46 V versus FeCp(2)(0/+1), followed by a product wave at E(1/2) = -1.83 V. Complex 4 also underwent irreversible reduction to uranium(iii) [E(pc) = -2.56 V], resulting in an irreversible product peak at E(pa) = -1.83 V. One-electron reduction of complexes 3 and 4 using K(naphthalenide) under an argon atmosphere in DME yielded 6-coordinate [(XA(2))UCl(DME)] (5) and the thermally unstable 7-coordinate [(TXA(2))U(DME)Cl(2)Li(DME)(2)] (6), respectively. The U-S distances in 4 and 6 are u...Continue Reading

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Citations

Aug 15, 2013·Environmental Science and Pollution Research International·Bojidarka Ivanova, Michael Spiteller
Feb 5, 2016·Journal of the American Chemical Society·Rami J BatriceMoris S Eisen
Dec 23, 2015·Inorganic Chemistry·Jee Eon KimEric J Schelter
Oct 14, 2014·Dalton Transactions : an International Journal of Inorganic Chemistry·Qian-Rui HuangNikolas Kaltsoyannis
Mar 16, 2018·Dalton Transactions : an International Journal of Inorganic Chemistry·Nicholas R AndreychukHilary A Jenkins
May 20, 2021·Chemical Communications : Chem Comm·Shanmugam RevathiTapas Ghatak

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