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1990 (1)
1Author    PeterG. Jones, Anke Meyer, Reinhard Schmutzler, FrauM. Prof, BeckeRequires cookie*
 Title    Uber die Darstellung neuer spirocyclischer N,N'-Dimethylsulfamid-substituierter Phosphorverbindungen und N,N'-DimethyIsulfamid-verbrückter Diphosphorverbindungen The Preparation of New Spirocyclic N,N'-Dimethylsulphamide-Substituted Phosphorus Compounds, and of Some N,N'-Dimethylsulphamide-Bridged Diphosphorus Compounds  
 Abstract    The reactions of 4-chloro-l,3,5,7-tetramethyl-2,2,6,6-tetraoxa-2,6-dithia-l,3,5,7-tetraaza-4x:'-phosphaspiro[3.3]heptane (1) with trimethylsilyl compounds and sodium azide led to a series of spirocyclic N,N'-dimethylsulphamide-substituted phosphoranes (2—5). The nature of the penta-aza-spirophosphorane (4) was confirmed by an X-ray crystal structure determination (C2/c, a = 991.8(4), b = 1185.6(6), c = 1224.9(5) pm ,ß= 108.64(3)°, Z = 4, R = 0.041 for 1065 unique observed reflections); a crystallographic twofold axis passes through phosphorus and the nitrogen atom of the NMe2 group. The geometry at phosphorus is to a good approximation trigonal bipyramidal. The azido-spirophosphorane (5) undergoes Staudinger-type reactions with phosphorus(III) com­ pounds (PPh3, dppm) to form the mixed-valence phosphorus compounds 6—8 . The reaction of N,N'-dimethylsulphamide or N,N'-dimethyl-N,N'-bis(trimethylsilyl)-sulphamide with dichloro-phosphines RPC12 (R = Me, Ph) in a molar ratio 1:2 leads to the formation of the acyclic N,N'-dimethylsulphamide-bridged diphosphorus compounds 9 and 10, respectively. The spectro­ scopic properties (and, for 4, the X-ray crystal structure) of the products are compared with those of analogous urea-bridged phosphorus compounds. 
  Reference    Z. Naturforsch. 45b, 175 (1990); eingegangen am 26. Juni/7. September 1989 
  Published    1990 
  Keywords    Spirophosphoranes, NN'-Dimethylsulphamide, X-Ray, Staudinger Reactions, Diphosphorus Compounds 
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 TEI-XML for    default:Reihe_B/45/ZNB-1990-45b-0175.pdf 
 Identifier    ZNB-1990-45b-0175 
 Volume    45