NEW RESULTS ON P4SE4

Autor(en): BLACHNIK, R
LONNECKE, P
NUSS, J
Stichwörter: Chemistry; Chemistry, Inorganic & Nuclear; GLASS; PHOSPHORUS-SELENIUM; PREPARATION; STRUCTURE, P-31-NMR; SULFUR; TETRAPHOSPHORUS TETRASELENIDE, P4SE4; TETRAPHOSPHORUS TRISELENIDE, P4SE3; THERMOCHEMISTRY
Erscheinungsdatum: 1994
Herausgeber: JOHANN AMBROSIUS BARTH VERLAG
Journal: ZEITSCHRIFT FUR ANORGANISCHE UND ALLGEMEINE CHEMIE
Volumen: 620
Ausgabe: 1
Startseite: 160
Seitenende: 166
Zusammenfassung: 
Preparation of P4Se4 from the elements yields always the beta-modification of P4Se4. Alpha-P4Se4 is obtained only with selenium deficient samples. However, it is also observed, when P4Se4 is annealed and then extracted with CS2. The insoluble part has the X-ray pattern of alpha-PSe4. A reversible alpha-beta transition is not observed. MAS-P-31-NMR investigations on solid P4Se4 by Eckert et al. [21 reveal P2Se4/2 building units, which are, in view of our results, not dimer but linked to a polymeric network. Well-crystallized samples of beta-P4Se4 are obtained only at measuring temperatures above 573 K. The structure is of monoclinic symmetry with the space group P2(1)/n (a = 1141.9, b = 729.0, c = 1211.0 pm, beta = 120.80-degrees). The reaction of alpha-P4Se3I2 with bis-(trimethyltin)selenide in CS2 at low temperature yields molecular alpha-P4Se4, which can be detected in solution by P-31-NMR spectroscopy. Alpha-P4Se4 has D2d-symmetry like alpha-P4S4. It polymerizes at higher temperature. Alpha-P4Se3I(SeSnMe3) and alpha-P4Se3(SeSnMe3)2 were observed in the course of this reaction, too. The analogous reaction of alpha-P4Se3I2 with bis-(trimethyltin)sulfide leads to comparable results.
ISSN: 00442313
DOI: 10.1002/zaac.19946200126

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