ISSN:
0009-2940
Keywords:
Heterosiloxanes
;
Stibinosiloxanes
;
Antimonites(III), silyl-, oxo-
;
NMR, solid-state
;
NMR; CPMAS
;
Chemistry
;
Inorganic Chemistry
Source:
Wiley InterScience Backfile Collection 1832-2000
Topics:
Chemistry and Pharmacology
Notes:
Treatment of Sb(OSiMe3)3 with NaOSiMe3 in the molar ratio 1:2 in hexane at ambient temperature leads to the formation of Me3SiOSiMe3 and a crystalline complex of the formula Na4[Sb2O(OSiMe3)8] in ca. 35% yield. The composition of the product has been confirmed by elemental analysis and negative-ion CI mass spectrometry. The single crystal X-ray structure analysis (rhombohedral, space group R\documentclass{article}\pagestyle{empty}\begin{document}$\bar{3}$\end{document}c, Z=6) resulted in a disorder model for the complex with pseudo-cubic symmetry owing to virtually random distribution of sodium and antimony atoms over the vertices of an oxygen-centered octahedron with the eight silyloxy groups capping the faces. Low solubility in non-coordinating solvents prevented solution NMR studies, but solid-state NMR investigations using cross polarization and magic-angle spinning techniques (13C, 29Si) allowed the assignment of a point group C2v structure with the SbIII atoms in cis position relative to the oxo center of the complex.
Additional Material:
4 Ill.
Type of Medium:
Electronic Resource
URL:
http://dx.doi.org/10.1002/cber.19931260415
Permalink
