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1Author    ThomasK. Aukorat, Reinhard SchmutzlerRequires cookie*
 Title    N,N',N'-Trimethylethylendiamin-substituierte Phosphor(III)-Verbindungen und deren Oxidation zu Derivaten mit tetra-und pentakoordiniertem Phosphor N,N',N'-Trim ethylethylenediam ine-Substituted Phosphorus(III) Com pounds and their Oxidation to Derivatives with Four-and Five-Coordinated Phosphorus  
 Abstract    A study was made o f the intramolecular donor-acceptor interaction in N ,N',N'-trim ethyl-ethylenediamine-substituted phosphorus com pounds, involving A3-, A4-and A5-phosphorus atom s, as a function o f the nature o f the substituents at phosphorus. The reaction o f N-trim ethylsilyl-N,N',N'-trim ethylethylenediam ine (1) with (Pr'0)2PCl furnished the acyclic, trimethylethylenediamine-substituted phosphorus(III) compound 4. There is no N M R spec­ troscopic evidence for an intramolecular donor-acceptor interaction between the phosphorus atom and the nitrogen atom o f the dim ethylam ino group in 4. The oxidation o f the trivalent phosphorus atom in 4 and in the related com pound 5 by sulfur, selenium, tetrachloro-o-benzoquinone, and hexafluoroacetone led to the corresponding A4P com pounds 6 -9 and to the A5P com pounds 10 and 11. N o intramolecular donor-acceptor interaction could be detected in any o f these products. There was no reaction between 5 and elemental tellurium. The reac­ tion products were characterized by N M R spectroscopy, mass spectrometry, and by elemental analysis. 
  Reference    Z. Naturforsch. 47b, 275 (1992); eingegangen am 29. August 1991 
  Published    1992 
  Keywords    N, N', N'-Trim ethylethylenediam ine, D o n o r-Acceptor Interaction, Oxidizing Agents, N M R Spectra, M ass Spectra 
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 TEI-XML for    default:Reihe_B/47/ZNB-1992-47b-0275.pdf 
 Identifier    ZNB-1992-47b-0275 
 Volume    47 
2Author    Thom As, K. Aukorat, PeterG. Jones, Reinhard SchmutzlerRequires cookie*
 Title    Das 7,8-Benzo-5-chloro-1,4,4-trimethyl-l-aza-4-azonia-6,9-dioxa-5 A5-phospha- spiro[4.4]nonanyl-Kation: Röntgenstrukturanalyse und temperaturabhängige ^ -N M R -Spektren4]nonanyl Cation: X-Ray Crystal Structure Determination and Variable 'H NMR Spectra  
 Abstract    The 7,8-Benzo-5-chloro-1,4,4-trimethyl-1 -aza-4-azonia-6,9-dioxa-5/l5-phosphaspiro[4. The 'H N M R spectrum o f the spirophosphorane 3 at room temperature indicates dynamic behaviour o f the cation. The low-temperature 'H N M R spectra o f 3 exhibit two sets o f dou­ blets for the protons o f the diastereotopic N (C H 3)2 groups. The free enthalpy o f activation for the dynamic process was determined (58.6 KJ/mole). In the reaction o f 3 with sodium tetra-phenylborate the crystalline com pound, 4, involving the non-coordinating anion, [B(C6H 5)4]~, was obtained. The X-ray crystal structure analysis o f 4 reveals the presence o f a five-membered ring, formally as a result o f intramolecular donor-acceptor interaction between the nitrogen atom o f the N (C H 3)2 group and phosphorus. The geometry at phosphorus deviates som ewhat from ideal trigonal bipyramidal. 
  Reference    Z. Naturforsch. 47b, 755 (1992); eingegangen am 9. September 1991 
  Published    1992 
  Keywords    N, N', N'-Trim ethylethylenediam ine, A zonium Salt, Donor-Acceptor-Interaction, Temperature-Dependent N M R Spectra, X-Ray Crystal Structure 
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 TEI-XML for    default:Reihe_B/47/ZNB-1992-47b-0755.pdf 
 Identifier    ZNB-1992-47b-0755 
 Volume    47 
3Author    Fausto Calderazzo, Guido Pam, M. Artin Sperrlea, Ulli EnglertbRequires cookie*
 Title    Electron-and Ligand-Transfer Reactions Involving N,N-Dialkylcarbamates. Synthesis and Molecular Structure of V jIf^ -C C sH ^ yC ^ C N t^ H ^ h  
 Abstract    Electron-and ligand-transfer reactions o f low-valent organom etallic com pounds o f titanium and vanadium with N,N-dialkylcarbam ates o f titanium(IV) are reported. The reaction o f VCp2 (Cp = ^-cyclopentadienyl) with T i(0 2C N E t2)4 affords, inter alia, the dimeric vana-dium(III) N ,N-diethylcarbam ato derivative V2Cp2(0 2C N E t2)4 which has been studied by X-ray diffraction methods. Crystal data; triclinic, space group P i; a = 10.802(2), b = 11.004(1), c = 8.960(1) Ä; a = 112.879(9), ß = 102.66(1), y = 102.42(1)°; V = 902.3(6) A 3; Z = 1; F(000) = 368, gcalc = 1.282 g em -3; n = 5.47 cm -1. It consists o f a centrosymmetric dimer, the two vanadium atom s being surrounded by four oxygen atom s o f the bridging N,N-diethylcar-bamato groups and by the cyclopentadienyl ligand. The metal atom exhibits a distorted square-pyramidal coordination geometry with the oxygen atom s occupying the basal plane. The reaction o f TiCp2(CO)2 or Vmes2 (mes = //6-l,3 ,5 -M e3C6H 3) with T i(0 2C N E t2)4 affords Ti(III) and V(III) N,N-diethylcarbam ato derivatives by a simultaneous ligand-and electron-transfer reaction. M agnesium N ,N-diisopropylcarbam ate, M g (0 2CNPr'2)2, has been obtained by a ligand-transfer reaction between M gCp2 and T i(0 2CNPr'2)3. 
  Reference    Z. Naturforsch. 47b, 389 (1992); received A ugust 9 / October 16 1991 
  Published    1992 
  Keywords    N, N-D ialkylcarbam ates, Vanadium, Titanium, Cyclopentadienyl, Electron Transfer 
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 TEI-XML for    default:Reihe_B/47/ZNB-1992-47b-0389.pdf 
 Identifier    ZNB-1992-47b-0389 
 Volume    47