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  • Chemistry  (6)
  • 1
    Electronic Resource
    Electronic Resource
    Die Kristall- und Molekülstruktur von S3N5PF2Frau Professor Margot Becke-Goehring zum 60. Geburtstage gewidmet (1974)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 406 (1974), S. 329-336 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal and Molecular Structure of S3N5PF2The structure of the title compound has been determined from three-dimensional X-ray data, by PATTERSON and FOURIER methods. Crystals are hexagonal, with unit cell dimensions a = 18.9l0, c = 5.302 A, space group R3m C3v5, and Z = 9. Least squares refinement, by use of 499 independent reflections measured on a diffractometer has reached R 4.3%.The structure is built of discrete SSN5PF2 molecules which can be looked upon as S4N4derivative: two opposite sulfur atoms are N-bridged and a third is substituted for a PF2-group. Contrary to a previously proposed structure1 the enviroment of phosphorus is tetrahedral. The now reported structure is in excellent agreement with chemical properties, mass-spectroscopie, and ESR-data.
    Notes: Die Struktur von S3N5PF3 wurde röntgenographisch bestimmt. Die Verbindung kristallisiert hexagonal in der Raumgruppe R3m-C3v5 mit a = 18,910, c = 5,302 Å und Z = 9. Die Verfeinerung nach der Methode der kleinsten Quadrate ergab einen R-Wert von 4,3%. Die Struktur der Molekel kann man sich abgeleitet denken vom S4N4 durch Verbrückung zweier sich gegenüberliegender Schwefelatome durch ein Stickstoff-Atom und Ersatz eines weiteren Schwefelatome durch eine PF2-Gruppe. Phosphor ist tetraedrisch koordiniert. Die gefundene Struktur steht in bester Übereinstimmung mit den chemischen Eigenschaften und den ESR- und massenspektroskopischen Befunden.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19744060228
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  • 2
    Electronic Resource
    Electronic Resource
    Hydrofluorierung von Bis(silylimido)tetramethyldiphosphoran (1977)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 429 (1977), S. 69-73 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Hydrofluorination of Bis(silylimido)tetramethyldiphosphoraneThe silylated bis(imidophosphorane), (CH3)2P[NSi(CH3)3]—P[NSi(CH3)3](CH3)2, 1 reacts in ether with hydrogen fluoride to give the tetrafluorodiphosphorane, (CH3)2PF2—PF2(CH3)2, 2, while hydrofluorination in fluorotrichloromethane gives the diazadiphosphetidin 3 and the iminophosphorane 4. The thermal decomposition of 2, studied by 19F and 31P-n.m.r. spectroscopy, yields trifluorodimethylphosphorane and tetramethyldiphosphane.
    Notes: Das silylierte Bis(imidophosphoran), (CH3)2P[NSi(CH3)3]—P[NSi(CH3)3] (CH3)2, 1 wird durch ätherischen Fluorwasserstoff in das Tetrafluordiphosphoran, (CH3)2PF2—PF2(CH3)2, 2 überführt, während die entsprechende. Hydrofluorierung in Fluortrichlormethan das N-Trimethylsilylfluordimethyl-diazadiphosphetidin 3 und Fluordichlormethyl-dimethyl-N(trimethylsilyl)iminophosphoran 4 liefert. 2 ist thermisch labil und zerfällt in Trifluordimethylphosphoran und Tetramethyldiphosphan.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19774290109
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  • 3
    Electronic Resource
    Electronic Resource
    Fluorierte Elementorganica: Oxidative Flüssigphasen-Direktfluorierung. X. Organyloxyfluorphosphorane: Direktsynthese durch F2-Addition an Phosphinic-, Phosphonic- sowie Phosphoricsäureester(fluoride) und ThermolyseverhaltenProfessor ROLF APPEL zum 60. Geburtstage am 25. Februar 1981 gewidmet. (1981)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 477 (1981), S. 59-70 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Fluorinated Organoelements: Oxidative Liquid-Phase Direct Fluorination. X. Organyloxyfluorophosphoranes: Direct Synthesis by F2-Addition to Phosphinic-, Phosphonic-, and Phosphoric-Acid Ester(fluorides) and Thermal BehaviourThe phenoxyfluorophosphoranes (PhO)2PF2R (2a: R = CH3, 2b: R = Ph) and (PhO)3-nPFn+2 (4a: n = 0, 4b: n = 1, 4c: n = 2) were obtained in reasonable yield by direct fluorination of the corresponding organyloxy(fluoro)phosphanes for the first time. Contrary to 4c the intramolecular ligand exchange can be frozen up in 4b. The up to now unknown thermally unstable alkoxy-substituted difluorides (AlkO)3-PF2Rn (6a: Alk = CH3, R = Ph), n = 2; 6b: Alk = CH2CF3, R = Ph, n = 2; 6c: Alk = CH3, R = Ph, n = 1; 6d: Alk = CH3, n = 0) were isolated by low temperature F2-addition in pure substance, too. Their thermal decomposition (scrambling, CH3F-elimination) was cleared up for 6a as model substance and transferred to (CH3O)3PF2 6d Here the splitting of (CH3)2O under “Arbusov-conditions” is very surprising. The trigonal bipyramidal covalent structure of all organyloxyphosphoranes was confirmed by multinuclear 19F, 31P{1H}, 13C{1H}) NMR experiments.
    Notes: Die Phenoxyfluorphosphorane (PhO)2PF2R (2a: R = CH3, 2b: R = Ph und (PhO)3-nPFn+2 (4a: n = 0, 4b: n = 1, 4c: n = 2 werden in guter Ausbeute erstmals durch Direktfluorierung der korrespondierenden Organyloxy(fluor)phosphane erhalten. Im Gegensatz zu 4c läßt sich in 4b der intramolekulare Ligandenaustausch einfrieren. Die bisher nicht beschriebenen, thermolabilen alkoxy-substituierten Difluoride (AlkO)3-;nPF2Rn (6a: Alk = CH3, R = Ph, n = 2; 6b: Alk = CH2CF3, R = Ph, n = 2; 6c: Alk = CH3, R = Ph, n = 1; 6d: Alk = CH3, n = 0) lassen sich ebenfalls durch F2-Addition bei tiefer Temperatur in Reinsubstanz isolieren. Ihre thermische Zersetzung (Neuverteilung, CH3F-Eliminierung) wird an 6a als Modellsubstrat aufgeklärt und auf (CH3O)3PF2 6d übertragen, wobei die Bildung von (CH3)2O unter „Arbusov-Bedingungen“ überrascht. Die trigonal-bipyramidale Kovalenz-Struktur sämtlicher Organyloxyphosphorane wird durch kombinierte 19F-, 31P{1H}- und 13C{1H}-NMR-Untersuchungen bestätigt.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19814770607
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  • 4
    Electronic Resource
    Electronic Resource
    Characterization of isomeric [CH5P]+· and [C2H7P]+· radical cations and some [C2H6P]+ phosphonium ions in the gas phase by their collisional activation spectra (1983)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1983), S. 327-330 
    Details
    ISSN: 0030-493X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Collisional activation spectra were used to characterize isomeric ion structures for [CH5P]+· and [C2H7P]+· radical cations and [C2H6P]+ even-electron ions. Apart from ionized methylphosphane, [CH3PH2]+·, ions of structure [CH2PH3]+· appear to be stable in the gas phase. Among the isomeric [C2H7P]+· ions stable ion structures [CH2PH2CH3]+· and [CH2CH2PH3]+·/[CH3CHPH3]+· are proposed as being generated by appropriate dissociative ionization reactions of alkyl phosphanes. At least three isomeric [C2H6]+ ions appear to exist, of which \documentclass{article}\pagestyle{empty}\begin{document}$ {\rm CH}_{\rm 3} - \mathop {\rm P}\limits^{\rm + } {\rm H = CH}_{\rm 2} $\end{document} could be identified positively.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/oms.1210180804
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  • 5
    Electronic Resource
    Electronic Resource
    Untersuchung der Umsetzung von Schwefel mit Natriumnitrit in DMF, DMSO und HMPT (1986)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 538 (1986), S. 177-190 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Investigation of the Reaction of Sulfur with Sodium Nitrite in DMF, DMSO, and HMPAThe mechanism of the title reaction has been elucidated by VIS/UV, IR, 15N NMR, and ESR spectrometric measurements, gas analysis, and chromatography. The course of the complex reaction and the great number of products  -  nitrous oxide, nitric oxide, sodium thiosulfate, sulfate, polysulfides, polythionates, nitrate  -  can be explained with the assumption that at first perthionitrates NaSxNO2 are formed, which are decomposed either to give dinitrogen monoxide and thiosulfate, or, react with nitrite to yield nitrate and perthionitrite NaS2NO which dissociates reversibly into sodium trisulfide(-I) and nitrogen monoxide. (The details of the two main series of competitive and consecutive reaction steps can be seen from the tabular summary at the end of the text). The characteristic colour change during the reaction from blue-Green to orange-red is due to the formation of the two coloured species: S3- (blue, λmax = 620 nm, g = 2.029) and ONSS- (red, λmax = 448 nm, δ(15N) = 334 ppm, ref. K15NO3).
    Notes: Durch VIS/UV-, IR-, 15N-NMR- und ESR-spektrometrische Messungen, sowie chromatographische und Gas-Analysen ist der Mechanismus der Titelreaktion aufgeklärt worden. Der Verlauf der komplexen Umsetzung und die groβe Anzahl von Produkten  -  Distickstoffoxid, Stickstoffmonoxid, Natriumthiosulfat, Sulfat, Polysulfide, Polythionate, Nitrat  -  können mit der Annahme erklärt werden, daß zunächst Natriumperthionitrate NaSxNO2 entstehen, die sich in Distickstoffoxid und Thiosulfat zersetzen, oder auch mit Nitrit zu Nitrat und Perthionitrit, NaSSNO, reagieren, das reversibel in Stickoxid und Natriumtrisulfid(1 - ) dissoziiert. (Bezüglich der Einzelheiten der konkurrierenden und aufeinander folgenden Reaktionsschritte vgl. Tab. 2.) Der charakteristische Farbwechsel während der Titelreaktion von blau-grün über braun nach orangerot ist auf die Entstehung zweier Farbträger zurückzuführen: S3- (blau, λmax = 620 nm, g = 2,029) und ONSS- (rot, λmax = 448 nm, δ(15N) = 334 ppm, bez. auf K15NO3).
    Additional Material: 8 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19865380718
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  • 6
    Electronic Resource
    Electronic Resource
    Darstellung silylierter Alkylen-bisiminophosphorane und ihre Cyclisierung mit Phosphor(V)-fluoridenFrau Professor Margot Becke-Goehring zum 60. Geburtstage gewidmet (1974)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 406 (1974), S. 131-144 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Preparation of Silylated Alkylene-Bisiminophosphoranes and the Cyclisation with Phosphorus(V) Fluorides thereofNew silylated bisiminophosphoranes of the type Ph2P(NSi(CH3)3)(CH2)n Ph2P(NSi(CH3)3) 2a, b and c (n = 1, 2, 3) and the similary structured cyclic siline 5 are prepared by reaction of the corresponding alkylene-bisphosphines with silylazides.Using etheric HCl, the opened chain compounds 2a and b, are desilylated; they undergo condensation reactions with fluorophosphoranes PhxPF5-x(x = 0, 1) - the same as 5 - splitting off fluorosilane forming the partially fluorinated ionic diphosphaza-phosphonium ring systems 7a, b and 8.
    Notes: Die Synthese neuartiger, silylierter Bisiminophosphorane des Typs Ph2P(NSi(CH3)3)—(CH2)(n)—PPh2(NSi(CH3)3) 2a, b und c mit n = 1, 2, 3 und des analog gebauten cyclischen Silins 5 erfolgt durch Umsetzung der betreffenden Alkylenbisphosphine mit Silylaziden. Die offenkettigen Vertreter 2a und b werden von ätherischer HCl desilyliert; sie kondensieren - ebenso wie 5 - mit den Fluorphosphoranen PhxPF5-x(x = 0, 1) unter Fluorsilanabspaltung zu den ionischen, partiell fluorierten Diphosphazaphosphonium-Ringsystemen 7a, b und 8. Die Identifizierung und Charakterisierung der Reaktionsprodukte erfolgt vor allem durch 19F- und 31P-NMR-Spektroskopie.
    Additional Material: 2 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19744060203
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