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Eight-membered rings of the composition [SO2(NR)2PR′]2 3a-d with R = CH3, C2H5, and R′ = CH3, C6H5, were prepared from substituted sulfamides and dichlorophosphanes in the presence of a tertiary amine. These molecules were characterized on the basis of 1H and 31P NMR investigations and of mass spectra. 3 a reacts with phosphorus pentachloride to yield the spirocyclic derivative 4 with the phosphorus atom in the center of two four-membered rings. Methyliodide reacts with 3 a and 3 b under opening of the eight- membered ring and formation of phosphonium salts. The structure of 3 b is discussed in detail. 8b crystallizes in the orthorhombic space group Pna 21 with a = 12.60(0), b = 13.27(1), c = 12.62(4) Å.
Photoelectron (PE) spectra of ethylene and vinylene carbonates and thiocarbonates as well as of methylene trithiocarbonate and some open-chain derivatives are reported.
The low energy bands, well separated in the unsaturated compounds, are assigned to lone pair and π type ionizations. The assignment is based on comparison of PE spectra, modified CNDO calculations, and sulfur Κβ emission spectra. The pronounced substituent effects due to which the first ionization potential varies from 8.4 eV to 11.1 eV are discussed.
Two routes for the preparation of (CH3)2SnS2N2 are given, which are kinetically controlled reactions. The molecule (CH3)2SnS2N2 was characterized by X-ray analysis. It is an interesting starting material for the preparation of S2N2CO and S3N2O. The latter reacts with iminosulfur oxides and isocyanates under the formation of S3N3SO2F and S3N3SO2CF3. The structure of S3N3SO2F was established by X-ray analysis. The bonding properties are discussed.
The cleavage of thin-nitrogen derivatives with S3N2Cl2 yields also five membered sulfurnitrogen rings. The structure and properties of P3N3F5NS3N2 and C3N3F2NS3N2 are reported. Six, eight and ten membered rings are formed by the reactions of (CH3)3Si–N = S = N–Si (CH3)3 with FSO2–N=S=O, these are S4N4O2 and S5N5+S3N3O4, respectively. The cation S5N5+ is a planar molecule, while the oxygen containing species are puckered. In S4N4O2 the oxygens are attached to one sulfur atom, which has a tetrahedral configuration.
The structure of the silicon containing cyclic and bicyclic rings (CH3)2Si(NSN)2Si(CH3)2 and CH3Si(NSN)3SiCH3 were determined.