Please use this identifier to cite or link to this item:
http://hdl.handle.net/10773/6135
Title: | X-ray diffraction and solid-state NMR studies of a germanium binuclear complex |
Author: | Mafra, Luís Almeida Paz, Filipe A. Shi, Fa-Nian Rocha, João Trindade, Tito Fernandez, Christian Makal, Anna Wozniak, Krzysztof Klinowski, Jacek |
Keywords: | Coordination modes Germanium Hydrothermal synthesis NMR spectroscopy Organic–inorganic hybrid composites |
Issue Date: | Dec-2005 |
Publisher: | Wiley |
Abstract: | A compound formulated as (C4H12N2)[Ge2(pmida)2(OH)2]·4H2O (where pmida4 =N-(phosphonomethyl) iminodiacetate and C4H12N2 2+ =piperazinedium cation), containing the anionic [Ge2(pmida)2(OH)2]2 complex, has been synthesised by the hydrothermal approach and its structure determined by single-crystal X-ray diffraction analysis. Several high-resolution solid-state magic-angle spinning (MAS) NMR techniques, in particular two-dimensional 1H–X(13C,31P) heteronuclear correlation (HETCOR) and 1H–1H homonuclear correlation (HOMCOR) experiments incorporating a frequencyswitched Lee–Goldburg (FS-LG) decoupling scheme, have been employed for the first time in such a material. Using these tools in tandem affords an excellent general approach to study the structure of other inorganic–organic hybrids. We assigned the NMR resonances with the help of C···H and P···H internuclear distances obtained through systematic statistical analyses of the crystallographic data. The compound was further characterised by powder X-ray diffraction techniques, IR and Raman spectroscopy, and by elemental and thermal analyses (thermogravimetric analysis and differential scanning calorimetry). |
Peer review: | yes |
URI: | http://hdl.handle.net/10773/6135 |
DOI: | 10.1002/chem.200500281 |
ISSN: | 0947-6539 |
Appears in Collections: | CICECO - Artigos DQ - Artigos |
Files in This Item:
File | Description | Size | Format | |
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Chem. Eur. J. 2006, 12, 363 – 375.pdf | 1.21 MB | Adobe PDF |
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