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Updated: Jun 28, 2025
Synthesis of Nine-atom Deltahedral Zintl Ions of Germanium and their Functionalization with Organic Groups
Published on: February 11, 2012
M-Ge-Si thermolytic molecular precursors and models for germanium-doped transition metal sites on silica
James P Dombrowski1,2, Vidmantas Kalendra3, Micah S Ziegler1,2
1Department of Chemistry, University of California, Berkeley, Berkeley, CA, USA. tdtilley@berkeley.edu.
Abstract:
The synthesis, thermolysis, and surface organometallic chemistry of thermolytic molecular precursors based on a new germanosilicate ligand platform, -OGe[OSi(OBu)3]3, is described. Use of this ligand is demonstrated with preparation of complexes containing the first-row transition metals Cr, Mn, and Fe. The thermolysis and grafting behavior of the synthesized complexes, Fe{OGe[OSi(OBu)3]3}2 (FeGe), Mn{OGe[OSi(OBu)3]3}2(THF)2 (MnGe) and Cr{OGe[OSi(OBu)3]3}2(THF)2 (CrGe), was evaluated using a combination of thermogravimetric analysis; nuclear magnetic resonance (NMR), ultraviolet-visible (UV-Vis), and electron paramagnetic resonance (EPR) spectroscopies; and single-crystal X-ray diffraction (XRD). Grafting of the precursors onto SBA-15 mesoporous silica and subsequent calcination in air led to substantial changes in transition metal coordination environments and oxidation states, the implications of which are discussed in the context of low-coordinate and low oxidation state thermolytic molecular precursors.
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