title: X-ray diffraction and solid-state NMR studies of a germanium binuclear complex.
abstract: A compound formulated as (C4H12N2)[Ge2(pmida)2(OH)2] x 4 H2O (where pmida(4-) = 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 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).
authors.affiliation: Department of Chemistry, University of Aveiro, CICECO, 3810-193 Aveiro, Portugal.
authors.forename: Luís
authors.initials: L
authors.lastname: Mafra
authors.forename: Filipe A Almeida
authors.initials: FA
authors.lastname: Paz
authors.forename: Fa-Nian
authors.initials: FN
authors.lastname: Shi
authors.forename: João
authors.initials: J
authors.lastname: Rocha
authors.forename: Tito
authors.initials: T
authors.lastname: Trindade
authors.forename: Christian
authors.initials: C
authors.lastname: Fernandez
authors.forename: Anna
authors.initials: A
authors.lastname: Makal
authors.forename: Krzysztof
authors.initials: K
authors.lastname: Wozniak
authors.forename: Jacek
authors.initials: J
authors.lastname: Klinowski