Synthesis, crystal structure, and NMR spectroscopy of a 1,3,2λ5,4λ5-oxathiadiphosphetane
Haiko Beckmann
Institut für Analytische Chemie der Technischen Universität Dresden, Mommsenstr. 13, D-01062 Dresden, Germany
Search for more papers by this authorGisela Ohms
Institut für Analytische Chemie der Technischen Universität Dresden, Mommsenstr. 13, D-01062 Dresden, Germany
Search for more papers by this authorCorresponding Author
Gisbert Großmann
Institut für Analytische Chemie der Technischen Universität Dresden, Mommsenstr. 13, D-01062 Dresden, Germany
Institut für Analytische Chemie der Technischen Universität Dresden, Mommsenstr. 13, D-01062 Dresden, GermanySearch for more papers by this authorKerstin Krüger
Institut für Analytische Chemie der Technischen Universität Dresden, Mommsenstr. 13, D-01062 Dresden, Germany
Search for more papers by this authorKlaus Klostermann
Institut für Analytische Chemie der Technischen Universität Dresden, Mommsenstr. 13, D-01062 Dresden, Germany
Search for more papers by this authorVolker Kaiser
Institut für Anorganische und Analytische Chemie der Technischen Universität Clausthal, Paul-Ernst-Str. 4, D-38678 Clausthal-Zellerfeld, Germany
Search for more papers by this authorHaiko Beckmann
Institut für Analytische Chemie der Technischen Universität Dresden, Mommsenstr. 13, D-01062 Dresden, Germany
Search for more papers by this authorGisela Ohms
Institut für Analytische Chemie der Technischen Universität Dresden, Mommsenstr. 13, D-01062 Dresden, Germany
Search for more papers by this authorCorresponding Author
Gisbert Großmann
Institut für Analytische Chemie der Technischen Universität Dresden, Mommsenstr. 13, D-01062 Dresden, Germany
Institut für Analytische Chemie der Technischen Universität Dresden, Mommsenstr. 13, D-01062 Dresden, GermanySearch for more papers by this authorKerstin Krüger
Institut für Analytische Chemie der Technischen Universität Dresden, Mommsenstr. 13, D-01062 Dresden, Germany
Search for more papers by this authorKlaus Klostermann
Institut für Analytische Chemie der Technischen Universität Dresden, Mommsenstr. 13, D-01062 Dresden, Germany
Search for more papers by this authorVolker Kaiser
Institut für Anorganische und Analytische Chemie der Technischen Universität Clausthal, Paul-Ernst-Str. 4, D-38678 Clausthal-Zellerfeld, Germany
Search for more papers by this authorAbstract
From the crude product of the synthesis of the dithiadiphosphetane [RP(S)S]2 (with R = 2,4,6-iPr3C6H2), the trans-oxathiadiphosphetane 
has been isolated, C30H40OP2S3. X-ray structure analysis and mass spectroscopic investigations give unequivocal evidence for this structure: monoclinic, C2/c (no. 15), a = 13.066(8), b = 21.726(8), c = 12.070(6) Å, β = 103.54(10)°, V = 3331 Å3, Z = 4, and Dc = 1.158 g/cm3. The asymmetric unit consists of half the formula unit. Solid-state 31P NMR spectra give information about the chemical shift anisotropy. Results of IGLO calculations of the 31P nuclear magnetic shielding tensor agree satisfactorily with the experimental data. Monitoring the reaction of several dithiadiphosphetanes with benzophenone in solution by 31P NMR spectroscopy indicates that additional oxathiadiphosphetanes as well as thiotrimetaphosphonates are present. © 1996 John Wiley & Sons, Inc.
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