title: (1)H-(13)C-(29)Si triple resonance and REDOR solid-state NMR-A tool to study interactions between biosilica and organic molecules in diatom cell walls.
abstract: Triple resonance solid-state NMR experiments using the spin combination (1)H-(13)C-(29)Si are still rarely found in the literature. This is due to the low natural abundance of the two heteronuclei. Such experiments are, however, increasingly important to study hybrid materials such as biosilica and others. A suitable model substance, ideally labeled with both (13)C and (29)Si, is thus very useful to optimize the experiments before applying them to studies of more complex samples such as biosilica. Tetraphenoxysilane could be synthesized in an easy, two-step synthesis including double isotope labelling. Using tetraphenoxysilane, we established a (1)H-(13)C-(29)Si double CP-based HETCOR experiment and applied it to diatom biosilica from the diatom species Thalassiosira pseudonana. Furthermore, we carried out (1)H-(13)C{(29)Si} CP-REDOR experiments in order to estimate the distance between the organic matrix and the biosilica. Our experiments on diatom biosilica strongly indicate a close contact between polyamine-containing parts of the organic matrix and the silica. This corroborates the assumption that the organic matrix is essential for the control of the cell wall formation.
authors: Bioanalytical Chemistry, Technische Universität Dresden, 01062 Dresden, Germany.
authors: Dorothea
authors: D
authors: Wisser
authors: Bioanalytical Chemistry, Technische Universität Dresden, 01062 Dresden, Germany.
authors: Stephan I
authors: SI
authors: Brückner
authors: Inorganic Chemistry I, Technische Universität Dresden, 01062 Dresden, Germany.
authors: Florian M
authors: FM
authors: Wisser
authors: Bruker Biospin GmbH, Silberstreifen 4, 76287 Rheinstetten, Germany.
authors: Gerhard
authors: G
authors: Althoff-Ospelt
authors: Inorganic Chemistry I, Technische Universität Dresden, 01062 Dresden, Germany.
authors: Jürgen
authors: J
authors: Getzschmann
authors: Inorganic Chemistry I, Technische Universität Dresden, 01062 Dresden, Germany.
authors: Stefan
authors: S
authors: Kaskel
authors: Bioanalytical Chemistry, Technische Universität Dresden, 01062 Dresden, Germany. Electronic address: Eike.Brunner@chemie.tu-dresden.de.
authors: Eike
authors: E
authors: Brunner
mesh_terms: D002473:Cell Wall / Q000737:chemistry*; D017377:Diatoms / Q000166:cytology*; D009682:Magnetic Resonance Spectroscopy / Q000379:methods*; D008958:Models, Molecular; D008968:Molecular Conformation; D009930:Organic Chemicals / Q000737:chemistry*; D012822:Silicon Dioxide / Q000737:chemistry*
chemical_list: D009930:Organic Chemicals; D012822:Silicon Dioxide
keywords: (13)C{(29)Si} REDOR; Biomineralization; Diatom biosilica; Double CP; Tetraphenoxysilane; Triple resonance NMR