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Synthesis of Ba(II) analogs of Ln(II)-in-(2.2.2-cryptand) and layered hexagonal net Ln(II) complexes, [(THF)Cs(µ–η5:η5–C5H4SiMe3)3LnII]

https://doi.org/10.1016/j.poly.2021.115493

Huh, Daniel N.; Ciccone, Sierra R.; Moore, William N.G.; Ziller, Joseph W.; Evans, William J. (December 2021, Polyhedron)

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2.2.2-Cryptand complexes of neptunium( iii ) and plutonium( iii )

https://doi.org/10.1039/D1CC05904A

Goodwin, Conrad A.; Ciccone, Sierra R.; Bekoe, Samuel; Majumdar, Sourav; Scott, Brian L.; Ziller, Joseph W.; Gaunt, Andrew J.; Furche, Filipp; Evans, William J. (January 2022, Chemical Communications)

New coordination environments are reported for Np( iii ) and Pu( iii ) based on pilot studies of U( iii ) in 2.2.2-cryptand (crypt). The U( iii )-in-crypt complex, [U(crypt)I 2 ][I], obtained from the reaction between UI 3 and crypt, is treated with Me 3 SiOTf (OTf = O 3 SCF 3 ) in benzene to form the [U(crypt)(OTf) 2 ][OTf] complex. Similarly, the isomorphous Np( iii ) and Pu( iii ) complexes were obtained similarly starting from [AnI 3 (THF) 4 ]. All three complexes (1-An; An = U, Np, Pu) contain an encapsulated actinide in a THF-soluble complex. Absorption spectroscopy and DFT calculations are consistent with 5f 3 U( iii ), 5f 4 Np( iii ), and 5f 5 Pu( iii ) electron configurations.
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High-Resolution X-ray Photoelectron Spectroscopy of Organometallic (C ₅ H ₄ SiMe ₃ ) ₃ Ln ^III and [(C ₅ H ₄ SiMe ₃ ) ₃ Ln ^II ] ^1– Complexes (Ln = Sm, Eu, Gd, Tb)

https://doi.org/10.1021/jacs.1c06980

Huh, Daniel N.; Bruce, Jared P.; Ganesh Balasubramani, Sree; Ciccone, Sierra R.; Furche, Filipp; Hemminger, John C.; Evans, William J. (October 2021, Journal of the American Chemical Society)

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Synthesis of Ln ^II ‐in‐Cryptand Complexes by Chemical Reduction of Ln ^III ‐in‐Cryptand Precursors: Isolation of a Nd ^II ‐in‐Cryptand Complex

https://doi.org/10.1002/anie.202006393

Huh, Daniel N.; Ciccone, Sierra R.; Bekoe, Samuel; Roy, Saswata; Ziller, Joseph W.; Furche, Filipp; Evans, William J. (June 2020, Angewandte Chemie International Edition)

Abstract Lanthanide triflates have been used to incorporate Nd^IIIand Sm^IIIions into the 2.2.2‐cryptand ligand (crypt) to explore their reductive chemistry. The Ln(OTf)₃complexes (Ln=Nd, Sm; OTf=SO₃CF₃) react with crypt in THF to form the THF‐soluble complexes [Ln^III(crypt)(OTf)₂][OTf] with two triflates bound to the metal encapsulated in the crypt. Reduction of these Ln^III‐in‐crypt complexes using KC₈in THF forms the neutral Ln^II‐in‐crypt triflate complexes [Ln^II(crypt)(OTf)₂]. DFT calculations on [Nd^II(crypt)]²⁺], the first Nd^IIcryptand complex, assign a 4f⁴electron configuration to this ion.
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