Vanadium-lithium alkoxides: Synthesis, structure, spectroscopic characterisation and accidental degradation of silicone grease

Dayane M. Reis; Kátia Cristina M. Westrup; Giovana G. Nunes; Andersson Barison; Ronny R. Ribeiro; Eduardo L. de Sá; David L. Hughes; Jaísa F. Soares

doi:10.1590/S0103-50532009000400005

Vanadium-lithium alkoxides: Synthesis, structure, spectroscopic characterisation and accidental degradation of silicone grease

Dayane M. Reis, Kátia Cristina M. Westrup, Giovana G. Nunes, Andersson Barison, Ronny R. Ribeiro, Eduardo L. de Sá, David L. Hughes, Jaísa F. Soares

Research output: Contribution to journal › Article › peer-review

12 Citations (Scopus)

Abstract

Two complexes containing both vanadium and lithium, [V₆Li₁₀O₈(ONep)₁₄{OSi(Me)₂ (ONep)}₂] (1) and [V(ONep)₃(μ-ONep)₂Li(thf)₂] (2), Nep = neopentyl, Me = methyl and thf = tetrahydrofuran, have been isolated in high yield and characterised by a number of techniques including X-band electron paramagnetic resonance (EPR) and ²⁹Si{¹H} nuclear magnetic resonance (NMR) spectroscopies, magnetic susceptibility measurements and single crystal X-ray diffractometry. Despite the similar preparation conditions, the two products present remarkably distinctive structural features: complex 2 is a binuclear adduct of "V(ONep)₄" and "Li(ONep)(thf)₂", while 1 is a mixed-valence, 16-metal aggregate. The large molecular oxoalkoxide 1 also contains silanolate units, {OSi(Me₂)(ONep)} ^-, produced by nucleophilic attack of neopentoxide groups on Si-O bonds of silicone grease accidentally dissolved in the reaction media. Both products have promising applications in organic and inorganic synthesis, including the preparation of uncommon V-Li and/or Si containing oxides.

Original language	English
Pages (from-to)	613-626
Number of pages	14
Journal	Journal of the Brazilian Chemical Society
Volume	20
Issue number	4
DOIs	https://doi.org/10.1590/S0103-50532009000400005
Publication status	Published - 2009

Keywords

Alkoxide
Lithium
Neopentoxide
Silicone grease
Vanadium(IV)

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10.1590/S0103-50532009000400005Licence: CC BY-NC

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Reis, Dayane M. ; Westrup, Kátia Cristina M. ; Nunes, Giovana G. ; Barison, Andersson ; Ribeiro, Ronny R. ; de Sá, Eduardo L. ; Hughes, David L. ; Soares, Jaísa F. / Vanadium-lithium alkoxides: Synthesis, structure, spectroscopic characterisation and accidental degradation of silicone grease. In: Journal of the Brazilian Chemical Society. 2009 ; Vol. 20, No. 4. pp. 613-626.

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title = "Vanadium-lithium alkoxides: Synthesis, structure, spectroscopic characterisation and accidental degradation of silicone grease",

abstract = "Two complexes containing both vanadium and lithium, [V6Li10O8(ONep)14{OSi(Me)2 (ONep)}2] (1) and [V(ONep)3(μ-ONep)2Li(thf)2] (2), Nep = neopentyl, Me = methyl and thf = tetrahydrofuran, have been isolated in high yield and characterised by a number of techniques including X-band electron paramagnetic resonance (EPR) and 29Si{1H} nuclear magnetic resonance (NMR) spectroscopies, magnetic susceptibility measurements and single crystal X-ray diffractometry. Despite the similar preparation conditions, the two products present remarkably distinctive structural features: complex 2 is a binuclear adduct of {"}V(ONep)4{"} and {"}Li(ONep)(thf)2{"}, while 1 is a mixed-valence, 16-metal aggregate. The large molecular oxoalkoxide 1 also contains silanolate units, {OSi(Me2)(ONep)} -, produced by nucleophilic attack of neopentoxide groups on Si-O bonds of silicone grease accidentally dissolved in the reaction media. Both products have promising applications in organic and inorganic synthesis, including the preparation of uncommon V-Li and/or Si containing oxides.",

keywords = "Alkoxide, Lithium, Neopentoxide, Silicone grease, Vanadium(IV)",

author = "Reis, {Dayane M.} and Westrup, {K{\'a}tia Cristina M.} and Nunes, {Giovana G.} and Andersson Barison and Ribeiro, {Ronny R.} and {de S{\'a}}, {Eduardo L.} and Hughes, {David L.} and Soares, {Ja{\'i}sa F.}",

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doi = "10.1590/S0103-50532009000400005",

language = "English",

volume = "20",

pages = "613--626",

journal = "Journal of the Brazilian Chemical Society",

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}

Vanadium-lithium alkoxides: Synthesis, structure, spectroscopic characterisation and accidental degradation of silicone grease. / Reis, Dayane M.; Westrup, Kátia Cristina M.; Nunes, Giovana G.; Barison, Andersson; Ribeiro, Ronny R.; de Sá, Eduardo L.; Hughes, David L.; Soares, Jaísa F.

In: Journal of the Brazilian Chemical Society, Vol. 20, No. 4, 2009, p. 613-626.

Research output: Contribution to journal › Article › peer-review

TY - JOUR

T1 - Vanadium-lithium alkoxides: Synthesis, structure, spectroscopic characterisation and accidental degradation of silicone grease

AU - Reis, Dayane M.

AU - Westrup, Kátia Cristina M.

AU - Nunes, Giovana G.

AU - Barison, Andersson

AU - Ribeiro, Ronny R.

AU - de Sá, Eduardo L.

AU - Hughes, David L.

AU - Soares, Jaísa F.

PY - 2009

Y1 - 2009

N2 - Two complexes containing both vanadium and lithium, [V6Li10O8(ONep)14{OSi(Me)2 (ONep)}2] (1) and [V(ONep)3(μ-ONep)2Li(thf)2] (2), Nep = neopentyl, Me = methyl and thf = tetrahydrofuran, have been isolated in high yield and characterised by a number of techniques including X-band electron paramagnetic resonance (EPR) and 29Si{1H} nuclear magnetic resonance (NMR) spectroscopies, magnetic susceptibility measurements and single crystal X-ray diffractometry. Despite the similar preparation conditions, the two products present remarkably distinctive structural features: complex 2 is a binuclear adduct of "V(ONep)4" and "Li(ONep)(thf)2", while 1 is a mixed-valence, 16-metal aggregate. The large molecular oxoalkoxide 1 also contains silanolate units, {OSi(Me2)(ONep)} -, produced by nucleophilic attack of neopentoxide groups on Si-O bonds of silicone grease accidentally dissolved in the reaction media. Both products have promising applications in organic and inorganic synthesis, including the preparation of uncommon V-Li and/or Si containing oxides.

AB - Two complexes containing both vanadium and lithium, [V6Li10O8(ONep)14{OSi(Me)2 (ONep)}2] (1) and [V(ONep)3(μ-ONep)2Li(thf)2] (2), Nep = neopentyl, Me = methyl and thf = tetrahydrofuran, have been isolated in high yield and characterised by a number of techniques including X-band electron paramagnetic resonance (EPR) and 29Si{1H} nuclear magnetic resonance (NMR) spectroscopies, magnetic susceptibility measurements and single crystal X-ray diffractometry. Despite the similar preparation conditions, the two products present remarkably distinctive structural features: complex 2 is a binuclear adduct of "V(ONep)4" and "Li(ONep)(thf)2", while 1 is a mixed-valence, 16-metal aggregate. The large molecular oxoalkoxide 1 also contains silanolate units, {OSi(Me2)(ONep)} -, produced by nucleophilic attack of neopentoxide groups on Si-O bonds of silicone grease accidentally dissolved in the reaction media. Both products have promising applications in organic and inorganic synthesis, including the preparation of uncommon V-Li and/or Si containing oxides.

KW - Alkoxide

KW - Lithium

KW - Neopentoxide

KW - Silicone grease

KW - Vanadium(IV)

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U2 - 10.1590/S0103-50532009000400005

DO - 10.1590/S0103-50532009000400005

M3 - Article

AN - SCOPUS:70349142297

VL - 20

SP - 613

EP - 626

JO - Journal of the Brazilian Chemical Society

JF - Journal of the Brazilian Chemical Society

SN - 0103-5053

IS - 4

ER -

Vanadium-lithium alkoxides: Synthesis, structure, spectroscopic characterisation and accidental degradation of silicone grease

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