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
UR - http://www.scopus.com/inward/record.url?scp=0002872958&partnerID=8YFLogxK
U2 - 10.1016/0020-1693(95)04974-6
DO - 10.1016/0020-1693(95)04974-6
M3 - Article
AN - SCOPUS:0002872958
SN - 0020-1693
VL - 248
SP - 9
EP - 14
JO - Inorganica Chimica Acta
JF - Inorganica Chimica Acta
IS - 1
ER -