Benzoquinonoid-bridged dinuclear actinide complexes

Hohloch, Stephan; Pankhurst, James R.; Jaekel, Esther E.; Parker, Bernard F.; Lussier, Daniel J.; Garner, Mary E.; Booth, Corwin H.; Love, Jason B.; Arnold, John

doi:10.1039/c7dt02728a

Benzoquinonoid-bridged dinuclear actinide complexes

Journal Article · Wed Aug 23 00:00:00 EDT 2017 · Dalton Transactions

DOI:https://doi.org/10.1039/c7dt02728a· OSTI ID:1493246

^[1]; ^[2]; Jaekel, Esther E. ^[3]; ^[4]; Lussier, Daniel J. ^[4]; ^[4]; Booth, Corwin H. ^[5]; ^[6]; ^[4]

Univ. of California, Berkeley, CA (United States). Dept. of Chemistry; Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Chemical Sciences Division; Paderborn Univ. (Germany). Dept. of Chemistry
Univ. of California, Berkeley, CA (United States). Dept. of Chemistry; Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Chemical Sciences Division; Univ. of Edinburgh, Scotland (United Kingdom). EaStCHEM School of Chemistry
Univ. of California, Berkeley, CA (United States). Dept. of Chemistry
Univ. of California, Berkeley, CA (United States). Dept. of Chemistry; Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Chemical Sciences Division
Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Chemical Sciences Division
Univ. of Edinburgh, Scotland (United Kingdom). EaStCHEM School of Chemistry

We report here the coordination chemistry of the tripodal tris[2-amido(2-pyridyl)ethyl]amine ligand, L, with thorium(IV) and uranium(IV). Using a salt-metathesis strategy from the potassium salt of this ligand, K₃L, new actinide complexes were isolated, namely the dimeric thorium complex [ThCl(L)]₂ (1) and the monomeric uranium complex UI(THF)(L) (2); under different crystallisation conditions, the dimeric uranium complex is also isolated, [UI(L)]₂ (2-dimer). With the aim of studying electronic phenomena such as magnetic exchange between two actinide ions, we have synthesised the first examples of dinuclear, quinoid-bridged actinide complexes from dianionic 2,5-bis[2,6-(diisopropyl)anilide]-1,4-benzoquinone (Q^Dipp) and 2,5-bis[2-(methoxy)anilide]-1,4-benzoquinone (Q^OMe) ligands. The resulting complexes are [Th(L)]₂Q^Dipp (3), [Th(THF)(L)]₂Q^OMe (5) and [U(L)]₂Q^OMe (6). The targeted [U(L)]₂Q^Dipp complex (4) could not be isolated. All isolated complexes have been characterised by spectroscopic methods and X-ray crystallography. The uranium(IV) complexes 2-dimer and 6 have been studied by SQUID magnetometry but indicate that there is negligible magnetic exchange between the two uranium(IV) ions. The reduced form of 6, [K(18-c-6)][6^-] is unstable and highly sensitive, but X-ray crystallography indicates that it is a novel U^IVU^IV complex bridged by a quinoid-radical.

View Accepted Manuscript (DOE)

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

Sponsoring Organization:: Federal Ministry of Education and Research (BMBF) (Germany); German Academic Exchange Service (DAAD); National Inst. of Health (NIH) (United States); National Science Foundation (NSF) (United States); USDOE Office of Science (SC), Basic Energy Sciences (BES) (SC-22)

Grant/Contract Number:: AC02-05CH11231

OSTI ID:: 1493246

Journal Information:: Dalton Transactions, Journal Name: Dalton Transactions Journal Issue: 35 Vol. 46; ISSN 1477-9226

Publisher:: Royal Society of ChemistryCopyright Statement

Country of Publication:: United States

Language:: English

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Strongly coupled binuclear uranium–oxo complexes from uranyl oxo rearrangement and reductive silylation Arnold, Polly L.; Jones, Guy M.; Odoh, Samuel O. Nature Chemistry, Vol. 4, Issue 3 https://doi.org/10.1038/nchem.1270	journal	February 2012
Isolation and characterization of a uranium(VI)–nitride triple bond King, David M.; Tuna, Floriana; McInnes, Eric J. L. Nature Chemistry, Vol. 5, Issue 6 https://doi.org/10.1038/nchem.1642	journal	May 2013
A single molecule magnet behaviour in a D _3h symmetry Dy( iii ) complex involving a quinone–tetrathiafulvalene–quinone bridge Pointillart, Fabrice; Klementieva, Svetlana; Kuropatov, Viacheslav Chem. Commun., Vol. 48, Issue 5 https://doi.org/10.1039/C1CC16314K	journal	January 2012
Reactivity of uranium( iv ) bridged chalcogenido complexes U ^IV –E–U ^IV (E = S, Se) with elemental sulfur and selenium: synthesis of polychalcogenido-bridged uranium complexes Franke, Sebastian M.; Heinemann, Frank W.; Meyer, Karsten Chem. Sci., Vol. 5, Issue 3 https://doi.org/10.1039/C3SC52799A	journal	January 2014
Zero-field slow magnetic relaxation in a uranium( iii ) complex with a radical ligand Coutinho, Joana T.; Antunes, Maria A.; Pereira, Laura C. J. Chem. Commun., Vol. 50, Issue 71 https://doi.org/10.1039/C4CC04486J	journal	January 2014
Actinide-based single-molecule magnets Meihaus, Katie R.; Long, Jeffrey R. Dalton Transactions, Vol. 44, Issue 6 https://doi.org/10.1039/C4DT02391A	journal	January 2015
Radical anionic versus neutral 2,2′-bipyridyl coordination in uranium complexes supported by amide and ketimide ligands Diaconescu, Paula L.; Cummins, Christopher C. Dalton Transactions, Vol. 44, Issue 6 https://doi.org/10.1039/C4DT02422B	journal	January 2015
The role of 5f-orbital participation in unexpected inversion of the σ-bond metathesis reactivity trend of triamidoamine thorium( iv ) and uranium( iv ) alkyls Gardner, Benedict M.; Cleaves, Peter A.; Kefalidis, Christos E. Chem. Sci., Vol. 5, Issue 6 https://doi.org/10.1039/C4SC00182F	journal	January 2014
Exchange coupling and magnetic blocking in dilanthanide complexes bridged by the multi-electron redox-active ligand 2,3,5,6-tetra(2-pyridyl)pyrazine Demir, Selvan; Nippe, Michael; Gonzalez, Miguel I. Chem. Sci., Vol. 5, Issue 12 https://doi.org/10.1039/C4SC02154A	journal	January 2014
Uranium triamidoamine chemistry Gardner, Benedict M.; Liddle, Stephen T. Chemical Communications, Vol. 51, Issue 53 https://doi.org/10.1039/C5CC01360G	journal	January 2015
Improving f-element single molecule magnets Liddle, Stephen T.; van Slageren, Joris Chemical Society Reviews, Vol. 44, Issue 19 https://doi.org/10.1039/C5CS00222B	journal	January 2015
Neptunium and plutonium complexes with a sterically encumbered triamidoamine (TREN) scaffold Brown, Jessie L.; Gaunt, Andrew J.; King, David M. Chemical Communications, Vol. 52, Issue 31 https://doi.org/10.1039/C6CC01656A	journal	January 2016
An air stable radical-bridged dysprosium single molecule magnet and its neutral counterpart: redox switching of magnetic relaxation dynamics Dolinar, Brian S.; Gómez-Coca, Silvia; Alexandropoulos, Dimitris I. Chemical Communications, Vol. 53, Issue 14 https://doi.org/10.1039/C6CC09824J	journal	January 2017
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Assessing crystal field and magnetic interactions in diuranium-μ-chalcogenide triamidoamine complexes with U ^IV –E–U ^IV cores (E = S, Se, Te): implications for determining the presence or absence of actinide–actinide magnetic exchange Gardner, Benedict M.; King, David M.; Tuna, Floriana Chemical Science, Vol. 8, Issue 9 https://doi.org/10.1039/C7SC01998J	journal	January 2017
Uranium complexes supported by an aryloxide functionalised triazacyclononane macrocycle: synthesis and characterisation of a six-coordinate U(iii) species and insights into its reactivityElectronic supplementary information (ESI) available: synthetic and analytical results, including elemental analysis, for all new complexes, crystallographic information for 2 and 3, and computational details for 1, figures and tables. See http://www.rsc.org/suppdata/cc/b2/b208473b/ Castro-Rodriguez, Ingrid; Olsen, Kristian; Gantzel, Peter Chemical Communications, Issue 23 https://doi.org/10.1039/b208473b	journal	November 2002
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Isolation of a TMTAA‐Based Radical in Uranium bis‐TMTAA Complexes Hohloch, Stephan; Garner, Mary E.; Booth, Corwin H. Angewandte Chemie, Vol. 130, Issue 49 https://doi.org/10.1002/ange.201810971	journal	October 2018
Isolation of a TMTAA-Based Radical in Uranium bis-TMTAA Complexes Hohloch, Stephan; Garner, Mary E.; Booth, Corwin H. Angewandte Chemie International Edition, Vol. 57, Issue 49 https://doi.org/10.1002/anie.201810971	journal	November 2018
New supporting ligands in actinide chemistry: tetramethyltetraazaannulene complexes with thorium and uranium Hohloch, Stephan; Garner, Mary E.; Parker, Bernard F. Dalton Trans., Vol. 46, Issue 40 https://doi.org/10.1039/c7dt02682j	journal	January 2017
Structure and properties of [(4,6- ^t Bu ₂ C ₆ H ₂ O) ₂ Se] ₂ An(THF) ₂ , An = U, Np, and their reaction with p -benzoquinone Myers, Alexander J.; Rungthanaphatsophon, Pokpong; Behrle, Andrew C. Chemical Communications, Vol. 54, Issue 74 https://doi.org/10.1039/c8cc05244a	journal	January 2018
Structure and magnetism of a tetrahedral uranium( iii ) β-diketiminate complex Boreen, Michael A.; Gould, Colin A.; Booth, Corwin H. Dalton Transactions, Vol. 49, Issue 23 https://doi.org/10.1039/d0dt01599g	journal	January 2020

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CCDC 1510088: Experimental Crystal Structure Determination: WECVOS : bis(μ-chloro)-bis(N,N',N''-[nitrilotri(ethane-2,1-diyl)]tri(pyridin-2-amino))-di-thorium(iv) Hohloch, Stephan; Pankhurst, James R.; Jaekel, Esther E. https://doi.org/10.5517/ccdc.csd.cc1mpcj6 The current record is supplemented by this dataset	dataset	October 2016
CCDC 1510089: Experimental Crystal Structure Determination: WECVUY : bis(μ-iodo)-bis(N,N',N''-[nitrilotri(ethane-2,1-diyl)]tri(pyridin-2-amino))-di-uranium(iv) Hohloch, Stephan; Pankhurst, James R.; Jaekel, Esther E. https://doi.org/10.5517/ccdc.csd.cc1mpck7 The current record is supplemented by this dataset	dataset	October 2016
CCDC 1510091: Experimental Crystal Structure Determination: WECWAF : (μ-3,6-bis((2,6-diisopropylphenyl)imino)cyclohexa-1,4-diene-1,4-diolato)-bis(N,N',N''-[nitrilotri(ethane-2,1-diyl)]tri(pyridin-2-amino))-di-thorium(iv) unknown solvate Hohloch, Stephan; Pankhurst, James R.; Jaekel, Esther E. https://doi.org/10.5517/ccdc.csd.cc1mpcm9 The current record is supplemented by this dataset	dataset	January 2017
CCDC 1516433: Experimental Crystal Structure Determination: WECWUZ : iodo-(N,N',N''-[nitrilotri(ethane-2,1-diyl)]tri(pyridin-2-amino))-(tetrahydrofuran)-uranium tetrahydrofuran solvate Hohloch, Stephan; Pankhurst, James R.; Jaekel, Esther E. https://doi.org/10.5517/ccdc.csd.cc1mwz6p The current record is supplemented by this dataset	dataset	January 2017
CCDC 1526524: Experimental Crystal Structure Determination: WECWEJ : (μ-3,6-bis((2-methoxyphenyl)imino)cyclohexa-1,4-diene-1,4-diolato)-bis(N,N',N''-[nitrilotri(ethane-2,1-diyl)]tri(pyridin-2-amino))-di-uranium(iv) Hohloch, Stephan; Pankhurst, James R.; Jaekel, Esther E. https://doi.org/10.5517/ccdc.csd.cc1n7gq2 The current record is supplemented by this dataset	dataset	January 2017
CCDC 1526525: Experimental Crystal Structure Determination: WECWIN : (18-crown-6)-bis(tetrahydrofuran)-potassium (μ-3,6-bis((2-methoxyphenyl)imino)cyclohexa-1,4-diene-1,4-diolato)-bis(N,N',N''-[nitrilotri(ethane-2,1-diyl)]tri(pyridin-2-amino))-di-uranium tetrahydrofuran solvate Hohloch, Stephan; Pankhurst, James R.; Jaekel, Esther E. https://doi.org/10.5517/ccdc.csd.cc1n7gr3 The current record is supplemented by this dataset	dataset	January 2017
CCDC 1526526: Experimental Crystal Structure Determination: WECWOT : (μ-3,6-bis((2-methoxyphenyl)imino)cyclohexa-1,4-diene-1,4-diolato)-bis(N,N',N''-[nitrilotri(ethane-2,1-diyl)]tri(pyridin-2-amino))-bis(tetrahydrofuran)-di-thorium tetrahydrofuran solvate Hohloch, Stephan; Pankhurst, James R.; Jaekel, Esther E. https://doi.org/10.5517/ccdc.csd.cc1n7gs4 The current record is supplemented by this dataset	dataset	January 2017

Benzoquinonoid-bridged dinuclear actinide complexes

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