Abstract
An equimolar quantity of benzylpotassium and di-n-butylmagnesium were combined with three molar equivalents of diphenylamine in a solvent medium which consisted on THF, hexane and N,N,N',N',N ''-pentamethyldiethylenetriamine (PMDETA). This mixture produces a rare example of a potassium tris(amido) magnesiate, namely (PMDETA)center dot K(mu-NPh2)Mg(THF)(NPh2)(2) 1. Complex 1 was characterized by X-ray crystallography and H-1 and C-13 NMR spectroscopy. The solid state structure of 1 (particularly the metals' co-ordination spheres) differs considerably from that of previously characterized potassium magnesiates, presumably due to the less sterically demanding nature of the amido ligand employed in this study. The magnesium center is four-coordinate (usually three-coordinate in such ate systems) and as well as binding to three amido ligands, is coordinated to a THF molecule. Turning to the potassium center, it is bound to three N centers from the triamine PMDETA, only one amido group, and its coordination sphere is completed by a series of aryl-pi contacts. The H-1 NMR solution studies in C6D6 appear to show that the complex does not stay intact in arene but likely forms a solvent-separated species such as [K(C6D6)(x)](+)[(THF) Mg(NPh2)(3)].
| Language | English |
|---|---|
| Pages | 154-157 |
| Number of pages | 4 |
| Journal | Inorganica Chimica Acta |
| Volume | 384 |
| DOIs | |
| Publication status | Published - 1 Apr 2012 |
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Keywords
- structural elucidation
- tris(amido) potassium magnesiate
- spectroscopy
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}
Synthesis and structural elucidation of a rare example of a tris(amido) potassium magnesiate. / Fleming, Ben J.; Garcia-Alvarez, Pablo; Keating, Elizabeth; Kennedy, Alan; O'Hara, Charles.
In: Inorganica Chimica Acta, Vol. 384, 01.04.2012, p. 154-157.Research output: Contribution to journal › Article
TY - JOUR
T1 - Synthesis and structural elucidation of a rare example of a tris(amido) potassium magnesiate
AU - Fleming, Ben J.
AU - Garcia-Alvarez, Pablo
AU - Keating, Elizabeth
AU - Kennedy, Alan
AU - O'Hara, Charles
PY - 2012/4/1
Y1 - 2012/4/1
N2 - An equimolar quantity of benzylpotassium and di-n-butylmagnesium were combined with three molar equivalents of diphenylamine in a solvent medium which consisted on THF, hexane and N,N,N',N',N ''-pentamethyldiethylenetriamine (PMDETA). This mixture produces a rare example of a potassium tris(amido) magnesiate, namely (PMDETA)center dot K(mu-NPh2)Mg(THF)(NPh2)(2) 1. Complex 1 was characterized by X-ray crystallography and H-1 and C-13 NMR spectroscopy. The solid state structure of 1 (particularly the metals' co-ordination spheres) differs considerably from that of previously characterized potassium magnesiates, presumably due to the less sterically demanding nature of the amido ligand employed in this study. The magnesium center is four-coordinate (usually three-coordinate in such ate systems) and as well as binding to three amido ligands, is coordinated to a THF molecule. Turning to the potassium center, it is bound to three N centers from the triamine PMDETA, only one amido group, and its coordination sphere is completed by a series of aryl-pi contacts. The H-1 NMR solution studies in C6D6 appear to show that the complex does not stay intact in arene but likely forms a solvent-separated species such as [K(C6D6)(x)](+)[(THF) Mg(NPh2)(3)].
AB - An equimolar quantity of benzylpotassium and di-n-butylmagnesium were combined with three molar equivalents of diphenylamine in a solvent medium which consisted on THF, hexane and N,N,N',N',N ''-pentamethyldiethylenetriamine (PMDETA). This mixture produces a rare example of a potassium tris(amido) magnesiate, namely (PMDETA)center dot K(mu-NPh2)Mg(THF)(NPh2)(2) 1. Complex 1 was characterized by X-ray crystallography and H-1 and C-13 NMR spectroscopy. The solid state structure of 1 (particularly the metals' co-ordination spheres) differs considerably from that of previously characterized potassium magnesiates, presumably due to the less sterically demanding nature of the amido ligand employed in this study. The magnesium center is four-coordinate (usually three-coordinate in such ate systems) and as well as binding to three amido ligands, is coordinated to a THF molecule. Turning to the potassium center, it is bound to three N centers from the triamine PMDETA, only one amido group, and its coordination sphere is completed by a series of aryl-pi contacts. The H-1 NMR solution studies in C6D6 appear to show that the complex does not stay intact in arene but likely forms a solvent-separated species such as [K(C6D6)(x)](+)[(THF) Mg(NPh2)(3)].
KW - structural elucidation
KW - tris(amido) potassium magnesiate
KW - spectroscopy
UR - http://www.scopus.com/inward/record.url?scp=84857924756&partnerID=8YFLogxK
U2 - 10.1016/j.ica.2011.11.052
DO - 10.1016/j.ica.2011.11.052
M3 - Article
VL - 384
SP - 154
EP - 157
JO - Inorganica Chimica Acta
T2 - Inorganica Chimica Acta
JF - Inorganica Chimica Acta
SN - 0020-1693
ER -