X-ray diffraction and solid-state NMR studies of a germanium binuclear complex
authors Mafra, L; Paz, FAA; Shi, FN; Rocha, J; Trindade, T; Fernandez, C; Makal, A; Wozniak, K; Klinowski, J
nationality International
journal CHEMISTRY-A EUROPEAN JOURNAL
author keywords coordination modes; germanium; hydrothermal synthesis; NMR spectroscopy; organic-inorganic hybrid composites
keywords NUCLEAR-MAGNETIC-RESONANCE; HIGH-RESOLUTION NMR; ANGLE-SPINNING NMR; DIPOLAR-CORRELATION SPECTROSCOPY; MULTIPLE PULSE NMR; CROSS-POLARIZATION; CRYSTAL-STRUCTURES; N-(PHOSPHONOMETHYL)IMINODIACETIC ACID; MOLECULAR-STRUCTURE; LAYERED COMPOUNDS
abstract A compound formulated as (C4H12N2)[Ge-2(pmida)(2)(OH)(2)]center dot 4H(2)O (where pmida(4-) = N-(phosphonomethyl)iminodiacetate and C4H12N22+ = piperazinedium cation), containing the anionic [Ge-2(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 H-1-X(C-13,P-31) heteronuclear correlation (HETCOR) and H-1-H-1 homonuclear correlation (HOMCOR) experiments incorporating a frequency-switched Lee-Goldburg (FS-LG) decoupling scheme, have been employed for the first time in such a material. Using these tools in tandem affords an Keywords: coordination modes germanium - bydrothermal synthesis - NMR spectroscopy - organicinorganic hybrid composites excellent general approach to study the structure of other inorganic-organic hybrids. We assigned the NMR resonances with the help of C center dot center dot center dot H and P center dot center dot center dot 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).
publisher WILEY-V C H VERLAG GMBH
issn 0947-6539
year published 2006
volume 12
issue 2
beginning page 363
ending page 375
digital object identifier (doi) 10.1002/chem.200500281
web of science category Chemistry, Multidisciplinary
subject category Chemistry
unique article identifier WOS:000234453300004
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journal impact factor 4.857
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