A unique lithium halide complex, [(LiBr)2·3HMPA· toluene]: Synthesis from reaction of solid NH4Br with Bu nLi in HMPA (hexamethylphosphoramide)/toluene media, crystal structure showing two Li-Br units linked by three μ2-HMPA ligands, and detection of 7Li ⋯ 31P coupling in solutions of the complex

Donald Barr; Michael J. Doyle; Robert E. Mulvey; Paul R. Raithby; David Reed; Ronald Snaith; Dominic S. Wright

doi:10.1039/C39890000318

A unique lithium halide complex, [(LiBr)₂·3HMPA· toluene]: Synthesis from reaction of solid NH₄Br with Bu ⁿLi in HMPA (hexamethylphosphoramide)/toluene media, crystal structure showing two Li-Br units linked by three μ₂-HMPA ligands, and detection of ⁷Li ⋯ ³¹P coupling in solutions of the complex

Donald Barr
, Michael J. Doyle
, Robert E. Mulvey
, Paul R. Raithby
, David Reed
, Ronald Snaith
, Dominic S. Wright

University of Cambridge
University of Strathclyde
Edinburgh Napier University

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

Abstract

Reaction of solid NH₄Br with BuⁿLi and HMPA (hexamethylphosphoramide) (1: 1: 2 ratio) in toluene produces (LiBr) ₂·3HMPA·toluene, (1), shown by X-ray crystallography to contain (LiBr)₂·3HMPA molecules whose two terminal Li-Br units are linked by three μ₂-HMPA ligands and with toluene molecules lying between these units in the lattice; in arene solutions, the (LiBr)₂·3HMPA units remain intact, giving rise in ⁷Li n.m.r. spectra to 1: 3: 3: 1 quartets caused by through-bond (O=P) coupling of each ⁷Li nucleus to three ³¹P(HMPA) centres.

Original language	English
Pages (from-to)	318-319
Number of pages	2
Journal	Journal of the Chemical Society, Chemical Communications
Issue number	5
DOIs	https://doi.org/10.1039/C39890000318
Publication status	Published - 1989

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Molecular Medicine

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Barr, D., Doyle, M. J., Mulvey, R. E., Raithby, P. R., Reed, D., Snaith, R., & Wright, D. S. (1989). A unique lithium halide complex, [(LiBr)₂·3HMPA· toluene]: Synthesis from reaction of solid NH₄Br with Bu ⁿLi in HMPA (hexamethylphosphoramide)/toluene media, crystal structure showing two Li-Br units linked by three μ₂-HMPA ligands, and detection of ⁷Li ⋯ ³¹P coupling in solutions of the complex. Journal of the Chemical Society, Chemical Communications, (5), 318-319. https://doi.org/10.1039/C39890000318

A unique lithium halide complex, [(LiBr)₂·3HMPA· toluene]: Synthesis from reaction of solid NH₄Br with Bu ⁿLi in HMPA (hexamethylphosphoramide)/toluene media, crystal structure showing two Li-Br units linked by three μ₂-HMPA ligands, and detection of ⁷Li ⋯ ³¹P coupling in solutions of the complex. / Barr, Donald; Doyle, Michael J.; Mulvey, Robert E. et al.
In: Journal of the Chemical Society, Chemical Communications, No. 5, 1989, p. 318-319.

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

Barr, D, Doyle, MJ, Mulvey, RE, Raithby, PR, Reed, D, Snaith, R & Wright, DS 1989, 'A unique lithium halide complex, [(LiBr)₂·3HMPA· toluene]: Synthesis from reaction of solid NH₄Br with Bu ⁿLi in HMPA (hexamethylphosphoramide)/toluene media, crystal structure showing two Li-Br units linked by three μ₂-HMPA ligands, and detection of ⁷Li ⋯ ³¹P coupling in solutions of the complex', Journal of the Chemical Society, Chemical Communications, no. 5, pp. 318-319. https://doi.org/10.1039/C39890000318

Barr D, Doyle MJ, Mulvey RE, Raithby PR, Reed D, Snaith R et al. A unique lithium halide complex, [(LiBr)₂·3HMPA· toluene]: Synthesis from reaction of solid NH₄Br with Bu ⁿLi in HMPA (hexamethylphosphoramide)/toluene media, crystal structure showing two Li-Br units linked by three μ₂-HMPA ligands, and detection of ⁷Li ⋯ ³¹P coupling in solutions of the complex. Journal of the Chemical Society, Chemical Communications. 1989;(5):318-319. doi: 10.1039/C39890000318

Barr, Donald ; Doyle, Michael J. ; Mulvey, Robert E. et al. / A unique lithium halide complex, [(LiBr)₂·3HMPA· toluene] : Synthesis from reaction of solid NH₄Br with Bu ⁿLi in HMPA (hexamethylphosphoramide)/toluene media, crystal structure showing two Li-Br units linked by three μ₂-HMPA ligands, and detection of ⁷Li ⋯ ³¹P coupling in solutions of the complex. In: Journal of the Chemical Society, Chemical Communications. 1989 ; No. 5. pp. 318-319.

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title = "A unique lithium halide complex, [(LiBr)2·3HMPA· toluene]: Synthesis from reaction of solid NH4Br with Bu nLi in HMPA (hexamethylphosphoramide)/toluene media, crystal structure showing two Li-Br units linked by three μ2-HMPA ligands, and detection of 7Li ⋯ 31P coupling in solutions of the complex",

abstract = "Reaction of solid NH4Br with BunLi and HMPA (hexamethylphosphoramide) (1: 1: 2 ratio) in toluene produces (LiBr) 2·3HMPA·toluene, (1), shown by X-ray crystallography to contain (LiBr)2·3HMPA molecules whose two terminal Li-Br units are linked by three μ2-HMPA ligands and with toluene molecules lying between these units in the lattice; in arene solutions, the (LiBr)2·3HMPA units remain intact, giving rise in 7Li n.m.r. spectra to 1: 3: 3: 1 quartets caused by through-bond (O=P) coupling of each 7Li nucleus to three 31P(HMPA) centres.",

author = "Donald Barr and Doyle, \{Michael J.\} and Mulvey, \{Robert E.\} and Raithby, \{Paul R.\} and David Reed and Ronald Snaith and Wright, \{Dominic S.\}",

year = "1989",

doi = "10.1039/C39890000318",

language = "English",

pages = "318--319",

journal = "Journal of the Chemical Society, Chemical Communications",

issn = "0022-4936",

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T1 - A unique lithium halide complex, [(LiBr)2·3HMPA· toluene]

T2 - Synthesis from reaction of solid NH4Br with Bu nLi in HMPA (hexamethylphosphoramide)/toluene media, crystal structure showing two Li-Br units linked by three μ2-HMPA ligands, and detection of 7Li ⋯ 31P coupling in solutions of the complex

AU - Barr, Donald

AU - Doyle, Michael J.

AU - Mulvey, Robert E.

AU - Raithby, Paul R.

AU - Reed, David

AU - Snaith, Ronald

AU - Wright, Dominic S.

PY - 1989

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N2 - Reaction of solid NH4Br with BunLi and HMPA (hexamethylphosphoramide) (1: 1: 2 ratio) in toluene produces (LiBr) 2·3HMPA·toluene, (1), shown by X-ray crystallography to contain (LiBr)2·3HMPA molecules whose two terminal Li-Br units are linked by three μ2-HMPA ligands and with toluene molecules lying between these units in the lattice; in arene solutions, the (LiBr)2·3HMPA units remain intact, giving rise in 7Li n.m.r. spectra to 1: 3: 3: 1 quartets caused by through-bond (O=P) coupling of each 7Li nucleus to three 31P(HMPA) centres.

AB - Reaction of solid NH4Br with BunLi and HMPA (hexamethylphosphoramide) (1: 1: 2 ratio) in toluene produces (LiBr) 2·3HMPA·toluene, (1), shown by X-ray crystallography to contain (LiBr)2·3HMPA molecules whose two terminal Li-Br units are linked by three μ2-HMPA ligands and with toluene molecules lying between these units in the lattice; in arene solutions, the (LiBr)2·3HMPA units remain intact, giving rise in 7Li n.m.r. spectra to 1: 3: 3: 1 quartets caused by through-bond (O=P) coupling of each 7Li nucleus to three 31P(HMPA) centres.

UR - https://www.scopus.com/pages/publications/37049089357

U2 - 10.1039/C39890000318

DO - 10.1039/C39890000318

M3 - Article

AN - SCOPUS:37049089357

SN - 0022-4936

SP - 318

EP - 319

JO - Journal of the Chemical Society, Chemical Communications

JF - Journal of the Chemical Society, Chemical Communications

IS - 5

ER -

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