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X‐ray Diffraction and Solid‐State NMR Studies of a Germanium Binuclear Complex
Author(s) -
Mafra Luís,
Almeida Paz Filipe A.,
Shi FaNian,
Rocha João,
Trindade Tito,
Fernandez Christian,
Makal Anna,
Wozniak Krzysztof,
Klinowski Jacek
Publication year - 2005
Publication title -
chemistry – a european journal
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 1.687
H-Index - 242
eISSN - 1521-3765
pISSN - 0947-6539
DOI - 10.1002/chem.200500281
Subject(s) - homonuclear molecule , heteronuclear molecule , crystallography , thermogravimetric analysis , chemistry , differential scanning calorimetry , raman spectroscopy , solid state nuclear magnetic resonance , magic angle spinning , x ray crystallography , crystal structure , magic angle , nuclear magnetic resonance spectroscopy , diffraction , materials science , molecule , stereochemistry , nuclear magnetic resonance , physics , organic chemistry , optics , thermodynamics
A compound formulated as (C 4 H 12 N 2 )[Ge 2 (pmida) 2 (OH) 2 ] ⋅ 4 H 2 O (where pmida 4− = N ‐(phosphonomethyl)iminodiacetate and C 4 H 12 N 2 2+ =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 1 H–X( 13 C, 31 P) heteronuclear correlation (HETCOR) and 1 H– 1 H 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 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).