Hydride oxidation from a titanium–aluminum bimetallic complex: insertion, thermal and electrochemical reactivity

Brown, Alexandra C.; Altman, Alison B.; Lohrey, Trevor D.; Hohloch, Stephan; Arnold, John

doi:10.1039/c7sc01835e

Title: Hydride oxidation from a titanium–aluminum bimetallic complex: insertion, thermal and electrochemical reactivity

Journal Article · Wed May 31 00:00:00 EDT 2017 · Chemical Science

DOI:https://doi.org/10.1039/c7sc01835e· OSTI ID:1399463

Brown, Alexandra C. ^[1]; Altman, Alison B. ^[2];

^[2];

^[2]

Univ. of California, Berkeley, CA (United States)
Univ. of California, Berkeley, CA (United States); Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States)

We report the synthesis and reactivity of paramagnetic heterometallic complexes containing a Ti(III)-μ-H-Al(III) moiety. Combining different stoichiometries amounts of Cp₂TiCl and KH₃AlC(TMS)₃ (Cp = cyclopentadienyl, TMS = trimethylsilyl) resulted in the formation of either bimetallic Cp₂Ti(μ-H)₂(H)AlC(TMS)₃ (2) or trimetallic (Cp₂Ti)₂(μ-H)₃(H)AlC(TMS)₃ (3) via salt metathesis pathways. While these complexes were indefinitely stable at room temperature, the bridging hydrides were readily activated upon exposure to heteroallenes, heating, or electrochemical oxidation. In each case, formal hydride oxidation occurred, but the isolated product maintained the +3 oxidation state at both metal centers. The nature of this reactivity was explored using deuterium labelling experiments and Density Functional Theory (DFT) calculations. It was found that while C–H activation from the Ti(III) bimetallic may occur through a σ-bond metathesis pathway, chemical oxidation to Ti(IV) promotes bimolecular reductive elimination of dihydrogen to form a Ti(III) product.

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

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

Grant/Contract Number:: AC02-05CH11231

OSTI ID:: 1399463

Journal Information:: Chemical Science, Vol. 8, Issue 7; ISSN 2041-6520

Publisher:: Royal Society of ChemistryCopyright Statement

Country of Publication:: United States

Language:: English

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Cited by: 15 works

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CCDC 1530362: Experimental Crystal Structure Determination: RAVDUQ : hexakis(μ-hydrido)-bis(tris(trimethylsilyl)methyl)-tetrakis(tetrahydrofuran)-di-aluminium-di-potassium Brown, Alexandra C.; Altman, Alison B.; Lohrey, Trevor D. https://doi.org/10.5517/ccdc.csd.cc1ncgj0 The current record is supplemented by this dataset	dataset	January 2017
CCDC 1530363: Experimental Crystal Structure Determination: RAVFAY : bis(μ-hydrido)-(η5-pentamethylcyclopentadienyl)-(η5-1-methanidyl-2,3,4,5-tetramethylcyclopentadienyl)-tris(trimethylsilyl)methyl-aluminium-titanium Brown, Alexandra C.; Altman, Alison B.; Lohrey, Trevor D. https://doi.org/10.5517/ccdc.csd.cc1ncgk1 The current record is supplemented by this dataset	dataset	January 2017
CCDC 1530364: Experimental Crystal Structure Determination: RAVFEC : tris(μ-hydrido)-bis(μ-η5-cyclopentadiendiyl)-bis (η5-cyclopentadienyl)-bis(tris(trimethylsilyl)methyl)-di-aluminium-di-titanium Brown, Alexandra C.; Altman, Alison B.; Lohrey, Trevor D. https://doi.org/10.5517/ccdc.csd.cc1ncgl2 The current record is supplemented by this dataset	dataset	January 2017
CCDC 1530365: Experimental Crystal Structure Determination: RAVFIG : tris(μ-fluoro)-tetrakis(η5-cyclopentadienyl)-tris(trimethylsilyl)methyl-fluoro-aluminium-di-titanium Brown, Alexandra; Altman, Alison; Lohrey, Trevor https://doi.org/10.5517/ccdc.csd.cc1ncgm3 The current record is supplemented by this dataset	dataset	January 2017
CCDC 1530366: Experimental Crystal Structure Determination: RAVFOM : tris(μ-hydrido)-hydrido-tetrakis(η5-cyclopentadienyl)-tris(trimethylsilyl)methyl-aluminium-di-titanium Brown, Alexandra C.; Altman, Alison B.; Lohrey, Trevor D. https://doi.org/10.5517/ccdc.csd.cc1ncgn4 The current record is supplemented by this dataset	dataset	January 2017
CCDC 1530367: Experimental Crystal Structure Determination: RAVFUS : (μ-oxo)-(N,N'-di-t-butyl-N-formylcarbamimidato)-bis(η5-cyclopentadienyl)-tris(trimethylsilyl)methyl-aluminium-titanium Brown, Alexandra C.; Altman, Alison B.; Lohrey, Trevor D. https://doi.org/10.5517/ccdc.csd.cc1ncgp5 The current record is supplemented by this dataset	dataset	January 2017
CCDC 1530368: Experimental Crystal Structure Determination: RAVGAZ : (μ-propan-2-yl[(propan-2-ylimino)methyl]amido)-(μ-hydrido)-bis(η5-cyclopentadienyl)-tris(trimethylsilyl)methyl-hydrido-aluminium-titanium Space Group: P 21/n (14), Cell: a 11.686(8)Å b 15.497(10)Å c 18.639(12)Å, α 90° β 107.884(5)° γ 90° Brown, Alexandra C.; Altman, Alison B.; Lohrey, Trevor D. https://doi.org/10.5517/ccdc.csd.cc1ncgq6 The current record is supplemented by this dataset	dataset	January 2017
CCDC 1530369: Experimental Crystal Structure Determination: RAVGED : (μ-hydrido)-(μ-trifluoromethanesulfonate)-bis(η5-cyclopentadienyl)-tris(trimethylsilyl)methyl-hydrido-aluminium-titanium Brown, Alexandra C.; Altman, Alison B.; Lohrey, Trevor D. https://doi.org/10.5517/ccdc.csd.cc1ncgr7 The current record is supplemented by this dataset	dataset	January 2017