TY - JOUR A1 - Kowalke, J. A1 - Arnold, C. A1 - Ponomarev, I. A1 - Jäger, Christian A1 - Kroll, P. A1 - Brendler, E. A1 - Kroke, E. T1 - Structural Insight into Layered Silicon Hydrogen Phosphates Containing [SiO6] Octahedra Prepared by Different Reaction Routes JF - European journal of inorganic chemistry N2 - The layered silicophosphate Si(HPO4)(2) was prepared via a novel synthesis approach using silicon nanopowder and ortho-phosphoric acid at 150 degrees C providing a polycrystalline product. Silicophosphate compounds with sixfold coordinated silicon atoms obtained from pyrophosphoric acid H4P2O7 and tetraalkoxysilanes via a sol-gel route exhibit the same short-range order. The solid products were analyzed with XRD, elemental analysis (ICP-AES), and detailed NMR spectroscopic studies, including H-1, C-13, Si-29, and P-31 MAS-, P-31-Si-29-REDOR, HETCOR, and CP-RFDR experiments. DFT calculations support the structure of Si(HPO4)(2) consisting of layers of [SiO6] octahedra linked by [O3P(OH)] tetrahedra. The OH groups point to the neighboring layers and may be substituted by ethoxy or other groups. KW - Silicon KW - Phosphorus KW - Sol-gel processes KW - NMR spectroscopy KW - Computational chemistry PY - 2019 DO - https://doi.org/10.1002/ejic.201801321 IS - 6 SP - 828 EP - 836 PB - ChemPubSoc AN - OPUS4-48058 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -