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Title: Chemical structure and bonding in a thorium( iii )–aluminum heterobimetallic complex

Journal Article · · Chemical Science
DOI:https://doi.org/10.1039/C8SC01260A· OSTI ID:1434399
 [1];  [2]; ORCiD logo [3]; ORCiD logo [1]; ORCiD logo [3];  [4]; ORCiD logo [5]; ORCiD logo [5]; ORCiD logo [1]
  1. Department of Chemistry, University of California, Berkeley, USA, Chemical Sciences Division
  2. Department of Chemistry, University of California, Berkeley, USA
  3. Department of Chemistry, University of California, Davis, USA
  4. LPCNO, Université de Toulouse, INAS Toulouse, Toulouse, France
  5. Chemical Sciences Division, Lawrence Berkeley National Laboratory, Berkeley, USA
+ Show Author Affiliations

Thorium sits at a unique position on the periodic table. On one hand, there is little evidence that its 5f orbitals engage in bonding as they do in other early actinides; on the other hand, its chemistry is distinct from Lewis acidic transition metals. To gain insight into the underlying electronic structure of Th and develop trends across the actinide series, it is useful to study Th(III) and Th(II) systems with valence electrons that may engage in non-electrostatic metal–ligand interactions, although only a handful of such systems are known. To expand the range of low-valent compounds and gain deeper insight into Th electronic structure, we targeted actinide bimetallic complexes containing metal–metal bonds. Here in this paper, we report the syntheses of Th–Al bimetallics from reactions between a di-tert-butylcyclopentadienyl supported Th(IV) dihalide (Cp‡2ThCl2) and an anionic aluminum hydride salt [K(H3AlC(SiMe3)3)]. Reduction of the [Th(IV)](Cl)–[Al] product resulted in a [Th(III)]–[Al] complex [Cp‡2Th(μ-H3)AlC(SiMe3)3]. The U(III) analogue [Cp‡2U(μ-H3)AlC(SiMe3)3] could be synthesized directly from a U(III) halide starting material. Electron paramagnetic resonance studies on 4 demonstrate hyperfine interactions between the unpaired electron and the Al atom indicative of spin density delocalization from the Th metal center to the Al. Density functional theory and atom in molecules calculations confirmed the presence of An→Al interactions in 4 and 5, which represents the first examples of An→M interactions where the actinide behaves as an electron donor.

Research Organization:
Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States)
Sponsoring Organization:
USDOE National Nuclear Security Administration (NNSA)
Grant/Contract Number:
AC02-05CH11231; NA0003180; NA0000979
OSTI ID:
1434399
Alternate ID(s):
OSTI ID: 1461125
Journal Information:
Chemical Science, Journal Name: Chemical Science Vol. 9 Journal Issue: 18; ISSN 2041-6520
Publisher:
Royal Society of Chemistry (RSC)Copyright Statement
Country of Publication:
United Kingdom
Language:
English
Citation Metrics:
Cited by: 24 works
Citation information provided by
Web of Science

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Formation of a Bridging Phosphinidene Thorium Complex journal November 2015
Use of 77 Se and 125 Te NMR Spectroscopy to Probe Covalency of the Actinide-Chalcogen Bonding in [Th(E n ){N(SiMe 3 ) 2 } 3 ] − (E = Se, Te; n = 1, 2) and Their Oxo-Uranium(VI) Congeners journal January 2016
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Elucidating bonding preferences in tetrakis(imido)uranate(VI) dianions journal April 2017
Ca(BH4)2 as a simple tool for the preparation of thorium and uranium metallocene borohydride complexes: First synthesis and crystal structure of (C5Me5)2Th(η3-H3BH)2 journal March 2017
Photochemical Route to Actinide-Transition Metal Bonds: Synthesis, Characterization and Reactivity of a Series of Thorium and Uranium Heterobimetallic Complexes journal February 2014
Covalency in f-element complexes journal January 2013
Bis(permethylindenyl) Complexes of Thorium:  Synthesis, Structure, and Reactivity journal July 2001
Synthesis of the First Tris(pentamethylcyclopentadienyl) Hydride Complex, (C 5 Me 5 ) 3 ThH journal December 2001
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The synthesis and characterisation, including X-ray diffraction study, of [Th{η-C 5 H 3 (SiMe 3 ) 2 } 3 ]; the first thorium( III ) crystal structure journal January 1986
Uranium-mediated activation of small molecules journal January 2011
Does Covalency Increase or Decrease across the Actinide Series? Implications for Minor Actinide Partitioning journal June 2012
A Linear, O-Coordinated  1-CO2 Bound to Uranium journal September 2004
Chloro-, methyl-, and (tetrahydroborato)tris((hexamethyldisilyl)amido)thorium(IV) and uranium(IV). Crystal structure of (tetrahydroborato)tris((hexamethyldisilyl)amido)thorium(IV) journal May 1979
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Evidence for the Involvement of 5f Orbitals in the Bonding and Reactivity of Organometallic Actinide Compounds: Thorium(IV) and Uranium(IV) Bis(hydrazonato) Complexes journal December 2008
[Al t Bu] −6: EPR Spectroscopic Evidence and Ab Initio Calculations journal October 1993
Trends in Covalency for d- and f-Element Metallocene Dichlorides Identified Using Chlorine K-Edge X-ray Absorption Spectroscopy and Time-Dependent Density Functional Theory journal September 2009
Electron-transfer and f-d absorption bands of some lanthanide and actinide complexes and the standard (II-III) oxidation potential for each member of the lanthanide and actinide series journal June 1973
A New Supporting Ligand in Actinide Chemistry Leads to Reactive Bis(NHC)borate-Supported Thorium Complexes journal August 2016
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Comparison of the Reactivity of 2-Li-C 6 H 4 CH 2 NMe 2 with MCl 4 (M=Th, U): Isolation of a Thorium Aryl Complex or a Uranium Benzyne Complex journal August 2013
Experimental and Computational Studies on the Formation of Thorium-Copper Heterobimetallics journal August 2016
Energy Decomposition Analysis of Metal−Metal Bonding in [M 2 X 8 ] 2- (X = Cl, Br) Complexes of 5f (U, Np, Pu), 5d (W, Re, Os), and 4d (Mo, Tc, Ru) Elements journal April 2007
A Thorium Chalcogenolate Series Generated by Atom Insertion into Thorium–Carbon Bonds journal April 2017
The vitality of uranium molecular chemistry at the dawn of the XXIst century journal January 2006
Preparation and Reactivity of the Versatile Uranium(IV) Imido Complexes U(NAr)Cl 2 (R 2 bpy) 2 (R = Me, t Bu) and U(NAr)Cl 2 (tppo) 3 journal August 2014
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Metal-metal bonds involving actinides. Synthesis and characterization of a complex having an unsupported actinide to transition metal bond journal December 1985
Synthesis, structure, and catalytic activity of an organothorium hydride complex journal November 2011
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Thorium Triamidoamine Complexes: Synthesis of an Unusual Dinuclear Tuck-in–Tuck-over Thorium Metallacycle Featuring the Longest Known Thorium−σ-Alkyl Bond journal November 2014
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Solution Structure and Behavior of Dimeric Uranium(III) Metallocene Halides journal March 1999
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Synthesis and x-ray structure of (C5Me5)2Th(.mu.-PPh2)2Pt(PMe3): a complex with a thorium-platinum bond journal January 1986
Probing the Coordinative Unsaturation and Local Environment of Ti 3+  Sites in an Activated High-Yield Ziegler-Natta Catalyst journal February 2015

Cited By (73)

CCDC 1822996: Experimental Crystal Structure Determination: GEVHEX : tris(μ-hydrido)-(tris(trimethylsilyl)methyl)-chloro-bis(1,3-bis(t-butyl)cyclopentadienyl)-thorium(iv)-aluminium Space Group: P 21/n (14), Cell: a 14.6013(10)Å b 16.3421(10)Å c 18.0401(11)Å, α 90° β 93.323(3)° γ 90° dataset February 2018
CCDC 1822997: Experimental Crystal Structure Determination: GEVHIB : tris(μ-hydrido)-hydrido-(tris(trimethylsilyl)methyl)-bis(1,3-bis(t-butyl)cyclopentadienyl)-thorium(iv)-aluminium dataset February 2018
CCDC 1822998: Experimental Crystal Structure Determination: GEVHOH : tris(μ-hydrido)-(tris(trimethylsilyl)methyl)-bis(1,3-bis(t-butyl)cyclopentadienyl)-thorium(iii)-aluminium dataset February 2018
CCDC 1822999: Experimental Crystal Structure Determination: GEVHUN : tris(μ-hydrido)-(tris(trimethylsilyl)methyl)-bis(1,3-bis(t-butyl)cyclopentadienyl)-uranium(iii)-aluminium dataset February 2018
[Al t Bu] −6: EPR Spectroscopic Evidence and Ab Initio Calculations journal October 1993
The Chemistry of the Actinide and Transactinide Elements. 3rd ed., 5 vols. Edited by Lester R. Morss, Norman M. Edelstein, Jean Fuger, and Joseph J. Katz. journal February 2007
Synthesis and Properties of a Fifteen-Coordinate Complex: The Thorium Aminodiboranate [Th(H3BNMe2BH3)4] journal March 2010
Comparison of the Reactivity of 2-Li-C 6 H 4 CH 2 NMe 2 with MCl 4 (M=Th, U): Isolation of a Thorium Aryl Complex or a Uranium Benzyne Complex journal August 2013
Synthesis and Characterization of a Uranium(II) Monoarene Complex Supported by δ  Backbonding journal May 2014
The Renaissance of Non-Aqueous Uranium Chemistry journal June 2015
Molecular Single-Bond Covalent Radii for Elements 1-118 journal January 2009
Experimental and Computational Studies on the Formation of Thorium-Copper Heterobimetallics journal August 2016
Dinitrogen Activation at Iron and Cobalt Metallalumatranes journal July 2013
Multiple Bonds Between Metal Atoms book January 2005
Expanding the chemistry of U3+ reducing agents journal April 2006
Covalency in f-element complexes journal January 2013
Synthesis, structure, and catalytic activity of an organothorium hydride complex journal November 2011
Ca(BH4)2 as a simple tool for the preparation of thorium and uranium metallocene borohydride complexes: First synthesis and crystal structure of (C5Me5)2Th(η3-H3BH)2 journal March 2017
A comparative study of the reactivity of Zr(IV), Hf(IV) and Th(IV) metallocene complexes: Thorium is not a Group IV metal after all journal October 2007
A New Supporting Ligand in Actinide Chemistry Leads to Reactive Bis(NHC)borate-Supported Thorium Complexes journal August 2016
The electronic structure of actinide-containing molecules: a challenge to applied quantum chemistry journal July 1991
Density Functional Theory Studies of the Electronic Structure of Solid State Actinide Oxides journal October 2012
Energy Decomposition Analysis of Metal−Metal Bonding in [M 2 X 8 ] 2- (X = Cl, Br) Complexes of 5f (U, Np, Pu), 5d (W, Re, Os), and 4d (Mo, Tc, Ru) Elements journal April 2007
Importance of Energy Level Matching for Bonding in Th 3+ -Am 3+ Actinide Metallocene Amidinates, (C 5 Me 5 ) 2 [ i PrNC(Me)N i Pr]An journal November 2010
Does Covalency Increase or Decrease across the Actinide Series? Implications for Minor Actinide Partitioning journal June 2012
Systematic Investigation of Thorium(IV)– and Uranium(IV)–Ligand Bonding in Dithiophosphonate, Thioselenophosphinate, and Diselenophosphonate Complexes journal August 2013
Preparation and Reactivity of the Versatile Uranium(IV) Imido Complexes U(NAr)Cl 2 (R 2 bpy) 2 (R = Me, t Bu) and U(NAr)Cl 2 (tppo) 3 journal August 2014
Chloro-, methyl-, and (tetrahydroborato)tris((hexamethyldisilyl)amido)thorium(IV) and uranium(IV). Crystal structure of (tetrahydroborato)tris((hexamethyldisilyl)amido)thorium(IV) journal May 1979
Electron-transfer and f-d absorption bands of some lanthanide and actinide complexes and the standard (II-III) oxidation potential for each member of the lanthanide and actinide series journal June 1973
Bonding of tris(.eta.5-cyclopentadienyl)-actinide complexes. 3. Interaction of .pi.-neutral, .pi.-acidic, and .pi.-basic ligands with (.eta.5-C5H5)3U journal April 1989
[Th(III)[.eta.5-C5H3(SiMe3)2]3], an actinide compound with a 6d1 ground state journal February 1988
Synthesis and x-ray structure of (C5Me5)2Th(.mu.-PPh2)2Pt(PMe3): a complex with a thorium-platinum bond journal January 1986
Metal-metal bonds involving actinides. Synthesis and characterization of a complex having an unsupported actinide to transition metal bond journal December 1985
Metal–Alane Adducts with Zero-Valent Nickel, Cobalt, and Iron journal December 2011
Revisiting the Chemistry of the Actinocenes [(η 8 -C 8 H 8 ) 2 An] (An = U, Th) with Neutral Lewis Bases. Access to the Bent Sandwich Complexes [(η 8 -C 8 H 8 ) 2 An(L)] with Thorium (L = py, 4,4′-bipy, t BuNC, R 4 phen) journal June 2013
Photochemical Route to Actinide-Transition Metal Bonds: Synthesis, Characterization and Reactivity of a Series of Thorium and Uranium Heterobimetallic Complexes journal February 2014
A Heterobimetallic Complex With an Unsupported Uranium(III)−Aluminum(I) Bond: (CpSiMe 3 ) 3 U−AlCp* (Cp* = C 5 Me 5 ) journal August 2008
Evidence for the Involvement of 5f Orbitals in the Bonding and Reactivity of Organometallic Actinide Compounds: Thorium(IV) and Uranium(IV) Bis(hydrazonato) Complexes journal December 2008
Trends in Covalency for d- and f-Element Metallocene Dichlorides Identified Using Chlorine K-Edge X-ray Absorption Spectroscopy and Time-Dependent Density Functional Theory journal September 2009
A Comparison of 4 f vs 5 f Metal−Metal Bonds in (CpSiMe 3 ) 3 M−ECp* (M = Nd, U; E = Al, Ga; Cp* = C 5 Me 5 ): Synthesis, Thermodynamics, Magnetism, and Electronic Structure journal September 2009
Synthesis and Characterization of the First Sandwich Complex of Trivalent Thorium:  A Structural Comparison with the Uranium Analogue journal July 1999
Thorium Mono- and Bis(imido) Complexes Made by Reprotonation of cyclo -Metalated Amides journal August 2015
Use of 77 Se and 125 Te NMR Spectroscopy to Probe Covalency of the Actinide-Chalcogen Bonding in [Th(E n ){N(SiMe 3 ) 2 } 3 ] − (E = Se, Te; n = 1, 2) and Their Oxo-Uranium(VI) Congeners journal January 2016
Formation of a Bridging Phosphinidene Thorium Complex journal November 2015
Expanding Thorium Hydride Chemistry Through Th 2+ , Including the Synthesis of a Mixed-Valent Th 4+ /Th 3+ Hydride Complex journal March 2016
Synthesis, Structure, and Reactivity of the Sterically Crowded Th 3+ Complex (C 5 Me 5 ) 3 Th Including Formation of the Thorium Carbonyl, [(C 5 Me 5 ) 3 Th(CO)][BPh 4 ] journal February 2017
A Thorium Chalcogenolate Series Generated by Atom Insertion into Thorium–Carbon Bonds journal April 2017
Bis(permethylindenyl) Complexes of Thorium:  Synthesis, Structure, and Reactivity journal July 2001
Synthesis of the First Tris(pentamethylcyclopentadienyl) Hydride Complex, (C 5 Me 5 ) 3 ThH journal December 2001
Actinide Metallocene Hydride Chemistry: C–H Activation in Tetramethylcyclopentadienyl Ligands to Form [μ-η 5 -C 5 Me 3 H(CH 2 )- κC ] 2– Tuck-over Ligands in a Tetrathorium Octahydride Complex journal October 2013
Thorium Triamidoamine Complexes: Synthesis of an Unusual Dinuclear Tuck-in–Tuck-over Thorium Metallacycle Featuring the Longest Known Thorium−σ-Alkyl Bond journal November 2014
Is Thorium a d Transition Metal or an Actinide? An Answer from a DFT Study of the Reaction between Pyridine N -Oxide and Cp 2 M(CH 3 ) 2 with M = Zr, Th, and U journal February 2009
Solution Structure and Behavior of Dimeric Uranium(III) Metallocene Halides journal March 1999
A delocalized arene-bridged diuranium single-molecule magnet journal April 2011
Isolation and characterization of a uranium(VI)–nitride triple bond journal May 2013
Actinide covalency measured by pulsed electron paramagnetic resonance spectroscopy journal December 2016
Elucidating bonding preferences in tetrakis(imido)uranate(VI) dianions journal April 2017
Thorium–phosphorus triamidoamine complexes containing Th–P single- and multiple-bond interactions journal September 2016
The vitality of uranium molecular chemistry at the dawn of the XXIst century journal January 2006
Uranium-mediated activation of small molecules journal January 2011
Actinide-based single-molecule magnets journal January 2015
Si–H addition followed by C–H bond activation induced by a terminal thorium imido metallocene: a combined experimental and computational study journal January 2014
Synthesis, structure, and reactivity of crystalline molecular complexes of the {[C 5 H 3 (SiMe 3 ) 2 ] 3 Th} 1− anion containing thorium in the formal +2 oxidation state journal January 2015
A Linear, O-Coordinated  1-CO2 Bound to Uranium journal September 2004
Molecular Structure of an Unusual Organoactinide Hydride Complex Determined Solely by Neutron Diffraction journal January 1979
Probing the Coordinative Unsaturation and Local Environment of Ti 3+  Sites in an Activated High-Yield Ziegler-Natta Catalyst journal February 2015
Manipulation of organoactinide coordinative unsaturation. Synthesis, structures, and reactivity of thorium hydrocarbyls and hydrides with chelating bis(tetramethylcyclopentadienyl) ancillary ligands journal August 1988
Sterically Demanding Aryloxides as Supporting Ligands in Organoactinide Chemistry. Synthesis, Structural Characterization, and Reactivity of Th(O-2,6- t -Bu 2 C 6 H 3 ) 2 (CH 2 SiMe 3 ) 2 and Formation of the Trimeric Thorium Hydride Th 3 H 6 (O-2,6- t -Bu 2 C 6 H 3 ) 6 journal January 1996
In search of tris(trimethylsilylcyclopentadienyl) thorium journal January 2019
Isolierung schwer fassbarer Komplexe mit einer Aluminium-Element-Mehrfachbindung: Am Horizont zeichnet sich eine neue Aluminiumchemie ab journal September 2018
Experimental Realisation of Elusive Multiple-Bonded Aluminium Compounds: A New Horizon in Aluminium Chemistry journal September 2018
Infrared Spectra of the HAnX and H 2 AnX 2 Molecules (An=Th and U, X=Cl and Br) in Argon Matrices Supported by Electronic Structure Calculations journal January 2019
Synthesis and Structure of Uranium‐Silylene Complexes journal February 2020

Linked Research (4)

Figures / Tables (7)

Scheme 1(p. 3)figure Scheme 1
Fig. 1(p. 4)figure Fig. 1
Fig. 2(p. 4)figure Fig. 2
Scheme 2(p. 4)figure Scheme 2
Table 1(p. 4)table Table 1
Fig. 3(p. 5)figure Fig. 3
Fig. 4(p. 6)figure Fig. 4

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