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Title: X-ray diffraction and solid-state NMR studies of a germanium binuclear complex
Author: Mafra, Luis
Paz, Filipe A. Almeida
Shi, Fa-Nian
Rocha, Joao
Trindade, Tito
Fernandez, Christian
Makal, Anna
Wozniak, Krzysztof
Klinowski, Jacek
Keywords: Coordination modes
Hydrothermal synthesis
NMR spectroscopy
Organic–inorganic hybrid composites
Issue Date: Dec-2005
Publisher: Wiley-VCH Verlag Berlin
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
DOI: 10.1002/chem.200500281
ISSN: 0947-6539
Appears in Collections:DQ - Artigos

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