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Article type: Research Article
Authors: Žák, Z. | Růžička, A. | Vičková, M. | Fröhlichová, L.
Affiliations: Department of Inorganic Chemistry, Masaryk University, Kotlářska 2, 611 37 Brno, Czech Republic, E-mail: [email protected]
Abstract: Trichlorophosphazo-N-sulfurylchloride Cl3PNS(O2)- C1 (1) reacts with [(CH3)3Si]2NR, R = H, CH3 to give its N-trimethylsilyl derivatives (CH3)3SiN(H)P(Cl2)NS(O2)Cl (2) and (CH3)3SiN(CH3)P(Cl2)NS(O2)Cl (3). At elevated temperatures (2) reacts with CH3CN under an intramolecular elimination of (CH3)3SiCl and a formation of 3,3-dichloro-5-methyl-6H-l,2,4,6,3-thiatriazaphosphinine-1,1-dioxide P(Cl2)NS(O2)N(H)C(CH3)N. All compounds were characterized by their 31P-NMR spectra and chemical analysis and their identity was established by their crystal structure determination. (2): Orthorhombic, S.G. P212121, with a = 9.425(2), b = 10.507(3), c = 12.803(5) Å,DX= 1.591 g/cm3, Z = 4, reflections collected 1796, final R = 0.0392; (3): Orthorhombic, S.G. P212121, with a = 6.275(2), b = 12.638(3), c = 16.759(7) Å, DX = 1.587 g/cm3, Z = 4, reflections collected 1816, final R = 0.0370; (4): Orthorhombic, S.G. Pna21, with a = 7.784 (2), b = 13.911(3), c = 7.413(1) Å, DX = 1.953 g/cm3, Z = 4, reflections collected 2558, final R = 0.0265.
DOI: 10.1080/10241229712331341294
Journal: Main Group Chemistry, vol. 2, no. 2, pp. 155-160, 1997
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