Controlled Redox Chemistry at Cerium within a Tripodal Nitroxide Ligand Framework

Bogart, Justin A.; Lippincott, Connor A.; Carroll, Patrick J.; Booth, Corwin H.; Schelter, Eric J.

doi:10.1002/chem.201502952

Title: Controlled Redox Chemistry at Cerium within a Tripodal Nitroxide Ligand Framework

Journal Article · Tue Oct 27 00:00:00 EDT 2015 · Chemistry - A European Journal

DOI:https://doi.org/10.1002/chem.201502952· OSTI ID:1378668

Bogart, Justin A. ^[1]; Lippincott, Connor A. ^[1]; Carroll, Patrick J. ^[1]; Booth, Corwin H. ^[2]; Schelter, Eric J. ^[1]

Univ. of Pennsylvania, Philadelphia, PA (United States). Dept. of Chemistry
Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Chemical Sciences Division

Ligand reorganization has been shown to have a profound effect on the outcome of cerium redox chemistry. Through the use of a tethered, tripodal, trianionic nitroxide ligand, [((2-tBuNOH)C ₆ H ₄ CH ₂ ) ₃ N] ^3- (TriNO _x ^3- ), controlled redox chemistry at cerium was accomplished, and typically reactive complexes of tetravalent cerium were isolated. These included rare cationic complexes [Ce(TriNO _x )thf][BAr ^F ₄ ], in which Ar ^F =3,5-(CF ₃ ) ₂ -C ₆ H ₃ , and [Ce(TriNO x )py][OTf] . A rare complete Ce-halide series, Ce(TriNO _x )X, in which X=F ^- , Cl ^- , Br ^- , I ^- , was also synthesized. We explored the solution chemistry of these complexes through detailed solution-phase electrochemistry and ¹H NMR experiments and showed a unique shift in the ratio of species with inner- and outer-sphere anions with size of the anionic X ^- group. DFT calculations on the series of calculations corroborated the experimental findings. Also, the use of a bulky and strongly donating tethered tripodal nitroxide ligand allowed the controlled redox chemistry at cerium. As a result, rare examples of cationic Ce IV complexes were synthesized and fully characterized. The full Ce-halide series supported by the tripodal ligand framework is also reported (see scheme).

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Research Organization:: Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States)

Sponsoring Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES)

Grant/Contract Number:: AC02-05CH11231; SC0006518

OSTI ID:: 1378668

Journal Information:: Chemistry - A European Journal, Vol. 21, Issue 49; ISSN 0947-6539

Publisher:: ChemPubSoc EuropeCopyright Statement

Country of Publication:: United States

Language:: English

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37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
cerium
density functional calculations
electrochemistry
nitroxides
redox chemistry

Title: Controlled Redox Chemistry at Cerium within a Tripodal Nitroxide Ligand Framework

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