Synthesis and structure of [Bi2(NtBu)4]2Li 2·2THF; a bimetallic cubane fragment containing a [Bi2(NtBu)4]2- anion

Andrew J. Edwards; Michael A. Beswick; Jane R. Galsworthy; Michael A. Paver; Paul R. Raithby; Moira Ann Rennie; Christopher A. Russell; Kerry L. Verhorevoort; Dominic S. Wright

doi:10.1016/0020-1693(95)04974-6

Synthesis and structure of [Bi₂(N^tBu)₄]₂Li ₂·2THF; a bimetallic cubane fragment containing a [Bi₂(N^tBu)₄]^2- anion

Andrew J. Edwards, Michael A. Beswick, Jane R. Galsworthy, Michael A. Paver, Paul R. Raithby, Moira Ann Rennie, Christopher A. Russell, Kerry L. Verhorevoort, Dominic S. Wright

University of Cambridge

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

39 Citations (SciVal)

Abstract

The imido-Bi complex [Bi₂(N^tBu)₄]Li₂ · 2THF (1) has been prepared by the in situ reaction of [(Me₂N)Bi(μ-N^tBu)]₂ with [^tBuNHLi] in toluene/THF solution. The complex has been characterised by elemental analysis, solid-state IR spectroscopy, ¹H NMR spectroscopy in solution, and by a low-temperature (153 K) X-ray diffraction study. The complex crystallises in the monoclinic space group P2₁/n, with cell dimensions a = 11.158(2), b = 16.777(3), c = 17.239(3) Å, β = 92.45(3)°, V = 3224.2(10) Å³ and Z = 4. Molecules of 1 consist of discrete [Bi₂Li₂N₄] cubane units in the solid state. Further association of these units into a structure akin to the previously characterised complex [Sb₂(NCy)₄]₂Li₄ (2), consisting of a cage of two interlocked 'broken cubes', is prevented by Lewis base solvation of Li. Solution NMR and cryoscopic studies of 2 show that the complex is involved in a dissociative equilibrium in which separate cubane units, similar to those identified in 1, are formed.

Original language	English
Pages (from-to)	9-14
Number of pages	6
Journal	Inorganica Chimica Acta
Volume	248
Issue number	1
DOIs	https://doi.org/10.1016/0020-1693(95)04974-6
Publication status	Published - 1 Jul 1996

Bibliographical note

Funding Information:
We gratefully acknowledge the EPSRC (M.A.B., A.J.E., JR.G., M.A.P., P.RR., C.A.R., K.L.V., D.S~W. ), 1.he Associated Octe! Co., Ltd., Ellesmere Port, UK (M.A.P., K.L.V., D.S.W.), the Royal Society (P.R.R., D.S.W.), the Nuffield Foundation (D.S.W.). and the Cambridge Crystallography Data Centre (M.A.R) for financial support.

Funding

We gratefully acknowledge the EPSRC (M.A.B., A.J.E., JR.G., M.A.P., P.RR., C.A.R., K.L.V., D.S~W. ), 1.he Associated Octe! Co., Ltd., Ellesmere Port, UK (M.A.P., K.L.V., D.S.W.), the Royal Society (P.R.R., D.S.W.), the Nuffield Foundation (D.S.W.). and the Cambridge Crystallography Data Centre (M.A.R) for financial support.

Keywords

Bismuth complexes
Crystal structures
Cubane complexes
Imido complexes

ASJC Scopus subject areas

Physical and Theoretical Chemistry
Inorganic Chemistry
Materials Chemistry

Access to Document

10.1016/0020-1693(95)04974-6

Cite this

@article{c9098665e88843239f62a2c1e426c280,

title = "Synthesis and structure of [Bi2(NtBu)4]2Li 2·2THF; a bimetallic cubane fragment containing a [Bi2(NtBu)4]2- anion",

abstract = "The imido-Bi complex [Bi2(NtBu)4]Li2 · 2THF (1) has been prepared by the in situ reaction of [(Me2N)Bi(μ-NtBu)]2 with [tBuNHLi] in toluene/THF solution. The complex has been characterised by elemental analysis, solid-state IR spectroscopy, 1H NMR spectroscopy in solution, and by a low-temperature (153 K) X-ray diffraction study. The complex crystallises in the monoclinic space group P21/n, with cell dimensions a = 11.158(2), b = 16.777(3), c = 17.239(3) {\AA}, β = 92.45(3)°, V = 3224.2(10) {\AA}3 and Z = 4. Molecules of 1 consist of discrete [Bi2Li2N4] cubane units in the solid state. Further association of these units into a structure akin to the previously characterised complex [Sb2(NCy)4]2Li4 (2), consisting of a cage of two interlocked 'broken cubes', is prevented by Lewis base solvation of Li. Solution NMR and cryoscopic studies of 2 show that the complex is involved in a dissociative equilibrium in which separate cubane units, similar to those identified in 1, are formed.",

keywords = "Bismuth complexes, Crystal structures, Cubane complexes, Imido complexes",

author = "Edwards, {Andrew J.} and Beswick, {Michael A.} and Galsworthy, {Jane R.} and Paver, {Michael A.} and Raithby, {Paul R.} and Rennie, {Moira Ann} and Russell, {Christopher A.} and Verhorevoort, {Kerry L.} and Wright, {Dominic S.}",

note = "Funding Information: We gratefully acknowledge the EPSRC (M.A.B., A.J.E., JR.G., M.A.P., P.RR., C.A.R., K.L.V., D.S~W. ), 1.he Associated Octe! Co., Ltd., Ellesmere Port, UK (M.A.P., K.L.V., D.S.W.), the Royal Society (P.R.R., D.S.W.), the Nuffield Foundation (D.S.W.). and the Cambridge Crystallography Data Centre (M.A.R) for financial support.",

year = "1996",

month = jul,

day = "1",

doi = "10.1016/0020-1693(95)04974-6",

language = "English",

volume = "248",

pages = "9--14",

journal = "Inorganica Chimica Acta",

issn = "0020-1693",

publisher = "Elsevier B.V.",

number = "1",

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TY - JOUR

T1 - Synthesis and structure of [Bi2(NtBu)4]2Li 2·2THF; a bimetallic cubane fragment containing a [Bi2(NtBu)4]2- anion

AU - Edwards, Andrew J.

AU - Beswick, Michael A.

AU - Galsworthy, Jane R.

AU - Paver, Michael A.

AU - Raithby, Paul R.

AU - Rennie, Moira Ann

AU - Russell, Christopher A.

AU - Verhorevoort, Kerry L.

AU - Wright, Dominic S.

N1 - Funding Information: We gratefully acknowledge the EPSRC (M.A.B., A.J.E., JR.G., M.A.P., P.RR., C.A.R., K.L.V., D.S~W. ), 1.he Associated Octe! Co., Ltd., Ellesmere Port, UK (M.A.P., K.L.V., D.S.W.), the Royal Society (P.R.R., D.S.W.), the Nuffield Foundation (D.S.W.). and the Cambridge Crystallography Data Centre (M.A.R) for financial support.

PY - 1996/7/1

Y1 - 1996/7/1

N2 - The imido-Bi complex [Bi2(NtBu)4]Li2 · 2THF (1) has been prepared by the in situ reaction of [(Me2N)Bi(μ-NtBu)]2 with [tBuNHLi] in toluene/THF solution. The complex has been characterised by elemental analysis, solid-state IR spectroscopy, 1H NMR spectroscopy in solution, and by a low-temperature (153 K) X-ray diffraction study. The complex crystallises in the monoclinic space group P21/n, with cell dimensions a = 11.158(2), b = 16.777(3), c = 17.239(3) Å, β = 92.45(3)°, V = 3224.2(10) Å3 and Z = 4. Molecules of 1 consist of discrete [Bi2Li2N4] cubane units in the solid state. Further association of these units into a structure akin to the previously characterised complex [Sb2(NCy)4]2Li4 (2), consisting of a cage of two interlocked 'broken cubes', is prevented by Lewis base solvation of Li. Solution NMR and cryoscopic studies of 2 show that the complex is involved in a dissociative equilibrium in which separate cubane units, similar to those identified in 1, are formed.

AB - The imido-Bi complex [Bi2(NtBu)4]Li2 · 2THF (1) has been prepared by the in situ reaction of [(Me2N)Bi(μ-NtBu)]2 with [tBuNHLi] in toluene/THF solution. The complex has been characterised by elemental analysis, solid-state IR spectroscopy, 1H NMR spectroscopy in solution, and by a low-temperature (153 K) X-ray diffraction study. The complex crystallises in the monoclinic space group P21/n, with cell dimensions a = 11.158(2), b = 16.777(3), c = 17.239(3) Å, β = 92.45(3)°, V = 3224.2(10) Å3 and Z = 4. Molecules of 1 consist of discrete [Bi2Li2N4] cubane units in the solid state. Further association of these units into a structure akin to the previously characterised complex [Sb2(NCy)4]2Li4 (2), consisting of a cage of two interlocked 'broken cubes', is prevented by Lewis base solvation of Li. Solution NMR and cryoscopic studies of 2 show that the complex is involved in a dissociative equilibrium in which separate cubane units, similar to those identified in 1, are formed.

KW - Bismuth complexes

KW - Crystal structures

KW - Cubane complexes

KW - Imido complexes

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DO - 10.1016/0020-1693(95)04974-6

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