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

Erickson, Karla A.; Scott, Brian Lindley; Kiplinger, Jaqueline Loetsch

doi:10.1016/j.inoche.2017.01.019

Title: 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

Abstract

Here, calcium borohydride allows for the high-yielding synthesis of (C₅Me₅)2An(η³-H₃BH)₂ (An = Th, U) by reaction with (C₅Me₅)₂AnCl₂ (An = Th, U). While a preparative synthesis of (C₅Me₅)₂U(η³-H₃BH)₂ has been previously reported in the literature using K(C₅Me₅) and U(BH₄)₄, the use of Ca(BH₄)₂ is higher yielding and mild. Full characterization of the novel compound (C₅Me₅)₂Th(η³-H₃BH)₂ is presented.

Authors:

Erickson, Karla A. ^[1];

^[1];

^[1]

Los Alamos National Lab. (LANL), Los Alamos, NM (United States)

Publication Date:: Wed Jan 18 00:00:00 EST 2017

Research Org.:: Los Alamos National Lab. (LANL), Los Alamos, NM (United States)

Sponsoring Org.:: USDOE Laboratory Directed Research and Development (LDRD) Program

OSTI Identifier:: 1351990

Alternate Identifier(s):: OSTI ID: 1396374

Report Number(s):: LA-UR-17-20498
Journal ID: ISSN 1387-7003

Grant/Contract Number:: AC52-06NA25396

Resource Type:: Accepted Manuscript

Journal Name:: Inorganic Chemistry Communications

Additional Journal Information:: Journal Volume: 77; Journal Issue: C; Journal ID: ISSN 1387-7003

Publisher:: Elsevier

Country of Publication:: United States

Language:: English

Subject:: 37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY; borohydride; thorium; uranium; pentamethylcylopentadienyl; X-ray crystallography

Citation Formats


                    Erickson, Karla A., Scott, Brian Lindley, and Kiplinger, Jaqueline Loetsch. 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.  United States: N. p., 2017. 
Web.  doi:10.1016/j.inoche.2017.01.019.

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                    Erickson, Karla A., Scott, Brian Lindley, & Kiplinger, Jaqueline Loetsch. 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.  United States.  https://doi.org/10.1016/j.inoche.2017.01.019

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                    Erickson, Karla A., Scott, Brian Lindley, and Kiplinger, Jaqueline Loetsch. Wed .  
"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".  United States.  https://doi.org/10.1016/j.inoche.2017.01.019.  https://www.osti.gov/servlets/purl/1351990.

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@article{osti_1351990,

  title        = {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},

  author       = {Erickson, Karla A. and Scott, Brian Lindley and Kiplinger, Jaqueline Loetsch},

  abstractNote = {Here, calcium borohydride allows for the high-yielding synthesis of (C5Me5)2An(η3-H3BH)2 (An = Th, U) by reaction with (C5Me5)2AnCl2 (An = Th, U). While a preparative synthesis of (C5Me5)2U(η3-H3BH)2 has been previously reported in the literature using K(C5Me5) and U(BH4)4, the use of Ca(BH4)2 is higher yielding and mild. Full characterization of the novel compound (C5Me5)2Th(η3-H3BH)2 is presented.},

  doi          = {10.1016/j.inoche.2017.01.019},

  journal      = {Inorganic Chemistry Communications},

  number       = C,

  volume       = 77,

  place        = {United States},

  year         = {Wed Jan 18 00:00:00 EST 2017},

  month        = {Wed Jan 18 00:00:00 EST 2017}

}

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https://doi.org/10.1016/j.inoche.2017.01.019

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Cited by: 6 works

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Figures / Tables:

Figure 1: Molecular structure of (C₅Me₅)₂Th( $\eta^3$-H₃BH)₂ (1) with thermal ellipsoids projected at the 50% probability level. The methyl groups on the pentamethylcyclopentadienyl ligands have been omitted for clarity. The hydrogen atoms attached to boron were located on the Fourier difference map and refined with restraints. Selected bond distances (Å)more »

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Works referenced in this record:

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Title: 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

Abstract

Citation Formats

Figures / Tables:

Synthesis, Structure, and Reactions of Hydride, Borohydride, and Aluminohydride Compounds of the f-Elements journal, October 1997

Covalent transition metal, lanthanide, and actinide tetrahydroborate complexes journal, April 1977

Arene uranium borohydrides: synthesis and crystal structure of η-C6Me6)U(BH4)3 journal, July 1989

New Chemistry from an Old Reagent: Mono- and Dinuclear Macrocyclic Uranium(III) Complexes from [U(BH 4 ) 3 (THF) 2 ] journal, July 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

Bis(permethylindenyl) Complexes of Thorium: Synthesis, Structure, and Reactivity journal, July 2001

Arene-ligated heteroleptic terphenolate complexes of thorium journal, January 2014

Tuning the Oxidation State, Nuclearity, and Chemistry of Uranium Hydrides with Phenylsilane and Temperature: The Case of the Classic Uranium(III) Hydride Complex [(C 5 Me 5 ) 2 U(μ-H)] 2 journal, February 2016

Phenylsilane as a safe, versatile alternative to hydrogen for the synthesis of actinide hydrides journal, January 2015

Synthesis of Cationic Cyclooctatetraene Uranium Complexes by Protonolysis of Borohydride Precursors: The First Cationic Organometallic Borohydride and the First Organometallic Dication of an f Element journal, June 2000

Uranium and Thorium Hydride Complexes as Multielectron Reductants: A Combined Neutron Diffraction and Quantum Chemical Study journal, February 2012

Reactivity of Tuck-in and Tuck-over Uranium Metallocene Complexes journal, September 2010

[(C5Me5)2U][(µ-Ph)2BPh2] as a four electron reductant journal, January 2005

Multi-Electron Reduction from Alkyl/Hydride Ligand Combinations in U 4+ Complexes journal, September 2008

Formal Three-Electron Reduction by an f-Element Complex: Formation of [{(C5Me5)(C8H8)U}2(C8H8)] from Cyclooctatetraene and [(C5Me5)3U] journal, January 2000

Reductive Coupling of Acetonitrile by Uranium and Thorium Hydride Complexes To Give Cyanopentadienyl Dianion (C6N3H7)2− journal, January 2008

Tetramethylphospholyluranium complexes and their pentamethylcyclopentadienyl analogues journal, February 1994

Some 60 new space-group corrections journal, January 2001

Novel hydroboration of highly substituted alkenes catalysed by borohydride complexes of uranium, neodymium and zirconium journal, January 1995

Synthesis and crystal structure of [UO2(BH4)2(hmpa)2], a novel uranyl complex and the first metal oxoborohydride journal, August 2007

Uranium(iv) amido-borohydrides as highly active diene polymerisation catalysts journal, January 2013

Title: 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

Synthesis, Structure, and Reactions of Hydride, Borohydride, and Aluminohydride Compounds of the f-Elements
journal, October 1997

Covalent transition metal, lanthanide, and actinide tetrahydroborate complexes
journal, April 1977

Arene uranium borohydrides: synthesis and crystal structure of η-C6Me6)U(BH4)3
journal, July 1989

New Chemistry from an Old Reagent: Mono- and Dinuclear Macrocyclic Uranium(III) Complexes from [U(BH ₄ ) ₃ (THF) ₂ ]
journal, July 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

Bis(permethylindenyl) Complexes of Thorium: Synthesis, Structure, and Reactivity
journal, July 2001

Arene-ligated heteroleptic terphenolate complexes of thorium
journal, January 2014

Tuning the Oxidation State, Nuclearity, and Chemistry of Uranium Hydrides with Phenylsilane and Temperature: The Case of the Classic Uranium(III) Hydride Complex [(C ₅ Me ₅ ) ₂ U(μ-H)] ₂
journal, February 2016

Phenylsilane as a safe, versatile alternative to hydrogen for the synthesis of actinide hydrides
journal, January 2015

Synthesis of Cationic Cyclooctatetraene Uranium Complexes by Protonolysis of Borohydride Precursors: The First Cationic Organometallic Borohydride and the First Organometallic Dication of an f Element
journal, June 2000

Uranium and Thorium Hydride Complexes as Multielectron Reductants: A Combined Neutron Diffraction and Quantum Chemical Study
journal, February 2012

Reactivity of Tuck-in and Tuck-over Uranium Metallocene Complexes
journal, September 2010

[(C5Me5)2U][(µ-Ph)2BPh2] as a four electron reductant
journal, January 2005

Multi-Electron Reduction from Alkyl/Hydride Ligand Combinations in U ⁴⁺ Complexes
journal, September 2008

Formal Three-Electron Reduction by an f-Element Complex: Formation of [{(C5Me5)(C8H8)U}2(C8H8)] from Cyclooctatetraene and [(C5Me5)3U]
journal, January 2000

Reductive Coupling of Acetonitrile by Uranium and Thorium Hydride Complexes To Give Cyanopentadienyl Dianion (C6N3H7)2−
journal, January 2008

Tetramethylphospholyluranium complexes and their pentamethylcyclopentadienyl analogues
journal, February 1994

Some 60 new space-group corrections
journal, January 2001

Novel hydroboration of highly substituted alkenes catalysed by borohydride complexes of uranium, neodymium and zirconium
journal, January 1995

Synthesis and crystal structure of [UO2(BH4)2(hmpa)2], a novel uranyl complex and the first metal oxoborohydride
journal, August 2007

Uranium(iv) amido-borohydrides as highly active diene polymerisation catalysts
journal, January 2013