Frau Professor Marianne Baudler zum 80. Geburtstag gewidmetInhaltsu È bersicht.1,3-Diselena-2,4-diphosphetan-2,4-diselenide, (RPSe 2 ) 2 , mit R = Me, Et, t-Bu, Ph, 4-Me 2 NC 6 H 4 , 4-MeOC 6 H 4 wurden nach verschiedenen Methoden hergestellt. Von den unlo È slichen Verbindungen wurden 31 P-und 77 Se-CP-MAS-Seitenbandspektren aufgenommen. Auf diese Weise konnte die Reinheit kontrolliert und an Hand der isotropen und anisotropen Werte der chemischen Verschiebungen sowie der Kopplungskonstanten 1 J P±Se die Struktur der untersuchten Verbindungen bewiesen werden. Auûerdem wurden zwei unter a È hnlichen Synthesebedingungen ent-stehende 1,2,4-Triselena-3,5-diphospholan-3,5-diselenide, (RPSe 2 ) 2 Se (R = Me, Et), untersucht, von denen die Struktur sowohl aus den 77 Se-Satelliten der 31 P-Lo È sungsspektren als auch aus Festko È rperspektren abgeleitet wurde. Am Beispiel von (t-BuPSe 2 ) 2 wurden die experimentell aus den Seitenbandspektren ermittelten Hauptachsenwerte der Phosphor-und Selen-Abschirmtensoren mit den aus IGLO-Berechnungen (HF und SOS-DFPT) erhaltenen Werten verglichen und die aus den Berechnungen ermittelten Hauptachsenlagen diskutiert. Abstract.1,3-Diselena-2,4-diphosphetane-2,4-diselenides (RPSe 2 ) 2 with R = Me, Et, t-Bu, Ph, 4-Me 2 NC 6 H 4 , 4-MeOC 6 H 4 have been synthesized by different methods. The insoluble compounds were investigated by 31 P and 77 Se solid-state NMR and the purity of the compounds has been checked by their CP MAS sideband NMR spectra. The structure of the investigated compounds has been confirmed by the isotropic and anisotropic values of the chemical shifts and the 1 J P±Se coupling constants. In addition, two new 1,2,4triselena-3,5-diphospholane-3,5-diselenides, (RPSe 2 ) 2 Se (R = Me, Et), formed under similar synthesis conditions, were investigated. Their structure was derived from the 77 Se satellites of 31 P solution spectra and from solid-state spectra. For (t-BuPSe 2 ) 2 the experimentally obtained principal values of phosphorus and selenium shielding tensors are compared with values from IGLO calculations (HF und SOS DFPT). The calculated orientations of the principal axes are discussed.

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The one-pot reaction of alkyl or aryl dichlorophosphanes RPCl 2 with alkali metal selenides M 2 Se and M 2 Se 2 in a 2:2:1 molar ratio provides a simple and general route to alkali metal tetraselenohypodiphosphonates (RP) 2 Se 4 M 2 (M = Li, Na; R = alkyl, aryl). The new compounds were characterized by multinuclear ( 31 P, 77 Se, 1 H, 13 C) NMR spectroscopy and

Mol­ecules of the title compound, C10H14O2, are connected by inter­molecular hydrogen bonds, forming zigzag chains running in the b‐axis direction. In addition, the two hydroxyl groups form an intra­molecular hydrogen bond.

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