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  • 1
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation, Crystal and Molecular Structure of Triphenylphosphineoxide Hydrochloride (C6H5)3PO · HCl(C6H5)3PO · HCl was prepared from HCl and (C6H5)3PO in benzene. It crystallizes in the monoclinic space group P21/n with a = 9.788(1), b = 16.477(6), c = 10.568(6) Å, β = 112.11(6)° and Z = 4; d(calc./obs.) 1,32/1,29 g · cm-3. The structure was determined by direct methods from 2 164 independent reflections and has been refined by full matrix least squares methods to R = 0.036. In the compound (C6H5)3PO and HCl are linked by a short, unsymmetrical, largely linear H-bond (distances O—Cl 2.747(2), O—H 1.116(40), H—Cl 1.633(40) Å, ∡ O—H—Cl 176.6(3.2)°). The P—O-distance measures 1.517(2) Å. From the position of the bridging H-Atom the compound can be conceived according to the contributing formula \documentclass{article}\pagestyle{empty}\begin{document}$ \left({{\rm C}_{\rm 6} {\rm H}_{\rm 5} } \right)_3 \mathop {\rm P}\limits^ + {\rm OH} \cdot \cdot \cdot \mathop {{\rm Cl}}\limits^ - $\end{document} as hydroxotriphenylphosphonium chloride.
    Notes: (C6H5)3PO · HCl wurde aus HCl und (C6H5)3PO in Benzol gewonnen. Es kristallisiert monoklin in der Raumgruppe P21/n mit a = 9,788(1), b = 16,477(6), c = 10,568(6) Å, β = 112,11(6)° und Z = 4; d(ber./gef.) = 1,32/1,29 g · cm-3. Die Struktur wurde anhand von 2 164 unabhängigen Reflexen direkt bestimmt und nach der Kleinste-Quadrate-Methode (volle Matrix) bis zu einem R-Wert von 0,036 verfeinert. In der Verbindung sind (C6H5)3PO und HCl über eine kurze unsymmetrische, weitgehend lineare H-Brücke (Abstände O—Cl 2,747(2), O—H 1,116(40), H—Cl 1,633(40) Å, ∡ O—H—Cl 176,6(3,2)°) verknüpft. Der P—O-Abstand beträgt 1,517(2) Å. Die Verbindung ist auf Grund der Lage des Brücken-H-Atoms entsprechend der Grenzstruktur \documentclass{article}\pagestyle{empty}\begin{document}$ \left({{\rm C}_{\rm 6} {\rm H}_{\rm 5} } \right)_3 \mathop {\rm P}\limits^ + {\rm OH} \cdot \cdot \cdot \mathop {{\rm Cl}}\limits^ - $\end{document} als Hydroxotriphenylphosphoniumchlorid aufzufassen.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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