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Preparation and Characterization of a Bis(silsesquioxane)tungsten Complex
Peter Smet1, Bart Devreese, Francis Verpoort
1Department of Inorganic and Physical Chemistry, Organometallics and Catalysis Division, University of Ghent, Krijgslaan 281 (S3), B-9000 Ghent, Belgium, Department of Biochemistry, Physiology and Microbiology, Laboratory of Protein Biochemistry and Protein Engineering, University of Ghent, K. L. Ledeganckstraat 35, B-9000 Ghent, Belgium, FG Strukturforschung, FB Materialwissenschaft, TU Darmstadt, Petersenstrasse 23, 64287 Darmstadt, Germany, and Institut für Organische Chemie, TU Darmstadt, Petersenstrasse 22, 64287 Darmstadt, Germany.
Abstract:
By reaction of tungsten(VI) chloride with the trisilanolic silsesquioxane (C(6)H(11))(7)Si(7)O(9)(OH)(3) (1), the bis(silsesquioxane)tungsten [(C(6)H(11))(7)Si(7)O(9)(O)(3)](2)W (3) complex is formed. This is evidenced by proton and carbon NMR and X-ray diffraction. Compound 3 crystallizes in the orthorhombic space group Cmca with a = 19.407(7) Å, b = 25.163(6) Å, c = 22.176(3) Å, V = 10829(5) Å(3), and Z = 4. In addition, the analysis of silsesquioxanes by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF), a technique initially developed for the characterization of biomolecules, has been successfully applied.