These tools will no longer be maintained as of December 31, 2024. Archived website can be found here. PubMed4Hh GitHub repository can be found here. Contact NLM Customer Service if you have questions.
Pubmed for Handhelds
PUBMED FOR HANDHELDS
Search MEDLINE/PubMed
Title: High-pressure synthesis and structural investigation of H3P8O8N9: a new phosphorus(V) oxonitride imide with an interrupted framework structure. Author: Sedlmaier SJ, Celinski VR, Schmedt auf der Günne J, Schnick W. Journal: Chemistry; 2012 Apr 02; 18(14):4358-66. PubMed ID: 22374911. Abstract: The first crystalline phosphorus oxonitride imide H(3)P(8)O(8)N(9) (=P(8)O(8)N(6)(NH)(3)) has been synthesized under high-pressure and high-temperature conditions. To this end, a new, highly reactive phosphorus oxonitride imide precursor compound was prepared and treated at 12 GPa and 750 °C by using a multianvil assembly. H(3)P(8)O(8)N(9) was obtained as a colorless, microcrystalline solid. The crystal structure of H(3)P(8)O(8)N(9) was solved ab initio by powder X-ray diffraction analysis, applying the charge-flipping algorithm, and refined by the Rietveld method (C2/c (no. 15), a=1352.11(7), b=479.83(3), c=1820.42(9) pm, β=96.955(4)°, Z=4). H(3)P(8)O(8)N(9) exhibits a highly condensed (κ=0.47), 3D, but interrupted network that is composed of all-side vertex-sharing (Q(4)) and only threefold-linking (Q(3)) P(O,N)(4) tetrahedra in a Q(4)/Q(3) ratio of 3:1. The structure, which includes 4-ring assemblies as the smallest ring size, can be subdivided into alternating open-branched zweier double layers {oB,2(2)(∞)}[(2)P(3)(O,N)(7)] and layers containing pairwise-linked Q(3) tetrahedra parallel (001). Information on the hydrogen atoms in H(3)P(8)O(8)N(9) was obtained by 1D (1)H MAS, 2D homo- and heteronuclear (together with (31)P) correlation NMR spectroscopy, and a (1)H spin-diffusion experiment with a hard-pulse sequence designed for selective excitation of a single peak. Two hydrogen sites with a multiplicity ratio of 2:1 were identified and thus the formula of H(3)P(8)O(8)N(9) was unambiguously determined. The protons were assigned to Wyckoff positions 8f and 4e, the latter located within the Q(3) tetrahedra layers.[Abstract] [Full Text] [Related] [New Search]