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'X Ray' in keywords Facet   Publication Year 1990  [X]
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1Author    Johannes Breker, PeterG. Jones, Reinhard Schmutzler, FrauM. Prof, Argot BeckeRequires cookie*
 Title    4-Substituierte  
 Abstract    ,3,5,7-T etramethyl-1,3,5,7-tetraaza-4 A5-phosphaspiro-|3.3]heptan-2,6-dione; Röntgenstrukturanalyse von 1,3,4,6,7,9,10-Heptamethyl-5-oxa-l ,3>7,9,10-pentaaza-4 A5,6 A5-diphosphadispiro[ ]decan-2,8-dion 4-Substituted l,3,5,7-Tetramethyl-l,3,5,7-tetraaza-4>3.5-phosphaspiro[3.3]heptane-2,6-diones; Crystal Structure of l,3,4,6,7,9,10-Heptamethyl-5-oxa-l,3,7,9,10-pentaaza-4A5, 6 / 5-diphospha-dispiro[3.1.3. l]decane-2,8-dione The reaction o f the tetrachlorophosphoranes RPC14 (R = Me, Ph) with N,N'-dimethylurea (dmh) (1), or o f the diazaphosphetidinone 0 = C (N M e)2PR (R = CC13) (3) and chlorine with N,N'-bis(trim ethylsilyl)-N,N'-dim ethylurea (2) furnished the spiro compounds 
  Reference    Z. Naturforsch. 45b, 1407—1415 (1990); eingegangen am 19. Oktober 1989 
  Published    1990 
  Keywords    Oxoazadiphosphetidine, N M R Spectroscopy, X-Ray 
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 TEI-XML for    default:Reihe_B/45/ZNB-1990-45b-1407.pdf 
 Identifier    ZNB-1990-45b-1407 
 Volume    45 
2Author    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 
3Author    N. Ullrich, C. Stegmair, H. Keller, E. Herdtweck, F. R. KreißlRequires cookie*
 Title    Darstellung und Struktur kationischer i^-Thiocarbenkomplexe von Molybdän und Wolfram Synthesis and Structure of Cationic //2-Thiocarbene Complexes of Molybdenum and Tungsten  
 Abstract    The reaction o f dim ethyl(m ethylthio)sulfonium tetrafluoroborate [(CH-,)-,S-SCH3][BF4] with //;'-cyclopentadienyl(dicarbonyl)carbyne com plexes o f molybdenum and tungsten Cp(CO)2M = C -R (M = M o. W; R = C H ,, C6H 5, C6H4C H 3) lc , 2 a ~ d results in an electrophilic attack o f the SCH, moiety at the metal carbon triple bond, providing orange to red, diam ag­ netic, cationic //--thiocarbene com plexes [Cp(CO):M = C(R)$CH,J[BF4] 3c, 4 a ~ d in high yields. The new com pounds were identified by X-ray structure analysis, N M R , IR and mass spectra. 
  Reference    Z. Naturforsch. 45b, 921 (1990); eingegangen am 9. November 1989 
  Published    1990 
  Keywords    Cationic ^-T hiocarbene Complexes, M olybdenum Tungsten, X-Ray 
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 TEI-XML for    default:Reihe_B/45/ZNB-1990-45b-0921.pdf 
 Identifier    ZNB-1990-45b-0921 
 Volume    45