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  • 1
    Publication Date: 2010-08-02
    Type: paper
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  • 2
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The electrochemical reduction of dialkylthallium(III) cations in aqueus buffer solutions and dimethylformamide yields by the first electron transfer the instable intermediate {R2Tl}, which in dependence of the reaction conditions is electrochemical reduced to Tl° or disproportionates to R3Tl and Tl°. Phenyl-substituted organothallium compounds are reduced to Tl° and (C6H5)2Hg in one step.
    Notes: Die elektrochemische Reduktion von Dialkylthallium(III)-Kationen in wäßrigen Puffersystemen und Dimethylformamid führt im Primärschritt zu {R2Tl}, das in Abhängigkeit von den Reaktionsbedingungen entweder elektrochemisch zu Tl° reduziert werden kann oder zu R3Tl und Tl° disproportioniert. Phenyl-substituierte Organothalliumverbindungen werden in DMF in einer Stufe zu Tl° und Diphenylquecksilber reduziert.
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  • 3
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: NMR Investigations on Dimeric Dialkylthallium Compoounds with (TIX)2 Four-membered Ring StructureNMR investigations on dimeric dialkylthallium amides and on dimethylthallium diphenylphosphide indicate a significant influence of the largeness of the bridging groups on the binding strength in the (TIX)2-four-membered ring structure. Exchange reactions among different dimeric dialkylthallium compounds give evidence of a dimer-monomer equilibrium, which is of fundamental importance for the reactivity and the reaction mechanisms of these compounds.
    Notes: NMR-Untersuchungen an dimeren Dialkylthalliumamiden und am Dimethylthalliumdiphenylphosphid indizieren einen signifikanten Einfluß der Größe der Brückengruppen auf die Bindungsstärke in den (TIX)2-Vierringen. Austauschreaktionen zwischen unterschiedlichen dimeren Dialkylthalliumverbindungen beweisen ein Dimer-Monomer-Gleichgewicht, das von grundsätzlicher Bedeutung für die Reaktivität und die Reaktionsmechanismen dieser Verbindungen ist.
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  • 4
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Secondary Phosphine Chalcogenides. X. Reactions of Diphenylphosphane Oxide, Ph2P(O)H, with the Bis(2,4-pentandionato) Complexes of Nickel, Palladium, and Platinum, Bis(cycloocta-1,5-diene)nickel(0) and Nickel Tetracarbonyl. Crystal and Molecular Structure of [Ni(acae) {(Ph2PO)2H}] (acac- = 0,0′-C5H7O2-)Reaction of [{Ni(acac)2}3] and [Pd(acac)2] with Ph2P(O)H yields [M(acac){(Ph2PO)2H}] (M = Ni, Pd) whereas [Pt(acac)2] results [Pt{(Ph2PO)2H}2]. The Nickel(0) complexes [Ni(cod)2] and [Ni(CO)4] react with Ph2P(O)H to give [Ni(cod)(Ph2PO)2] and [{Ni(μ-OPPh2)2}n], respectively. The IR and NMR spectra as well as some reactions of these complexes are described.The crystal structure of [Ni(acac){(Ph2PO)2H}] has been investigated by X-ray methods and refined to an R value of 0,099 (Rw = 0,088). The coordination geometry around the Ni atom is square planar with a slight tetrahedral distortion. The existence of a strong hydrogen bond within the (Ph2PO)2H- ligand is proved by the O…O distance at 237 pm.
    Notes: [{Ni(acac)2}3] und [Pd(acac)2] reagieren mit Ph2P(O)H zu [M(acac){(Ph2PO)2H}] (M = Ni, Pd), während [Pt(acac)2] [Pt{(Ph2PO)2H}2] ergibt. Die Nickel(0)-Komplexe [Ni(cod)2] und [Ni(CO)4] setzen sich mit Ph2P(O)H zu [Ni(cod)(Ph2PO)2] bzw. [{Ni(μ-OPPh2)2}n] um.Die IR- und NMR-Spektren dieser Komplexe und einige ihrer Reaktionen werden beschrieben.Die Kristallstruktur von [Ni(acac){(Ph2PO)2H}] wurde röntgenographisch bestimmt und bis zu einem R-Wert von 0,099 (Rw = 0,088) verfeinert. Die quadratisch-planare Koordinationsgeometrie um das Ni-Atom weist eine geringfügige tetraedrische Verzerrung auf. Das Vorliegen einer starken Wasserstoffbrückenbindung im (Ph2PO)2H--Liganden wird durch den O…O-Abstand von 237 pm bewiesen.
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  • 5
    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 Bis[1,2-bis(diphenylphosphino)ethane]nickel(O)The title compound [Ni(dppe)2] (dppe = Ph2PCH2CH2PPh2) crystallizes in the monoclinic space group P21/n with lattice parameters a = 983.2(2), b = 2119.2(3), c = 2145.1(4) pm, β = 91.97(1)°, and a unit cell contents of four molecules. The structure was solved by heavy atom method and refined to an R-value of 0.063 (RW = 0.052), using 2779 observed unique reflexions. The Ni atom as the spiro centre is distorted-tetrahedrally coordinated by the four P atoms of the two bidentate chelating ligands. The Ni—P bond lengths are very similar with a mean value of 216(1) pm. The mean value of Tolman's cone angle for the dppe ligand calculated from the molecular structure of [Ni(dppe)2] amounts to 129.8°.
    Notes: Die Titelverbindung [Ni(dppe)2] (dppe = Ph2PCH2CH2PPh2) kristallisiert in der monoklinen Raumgruppe P21/n mit den Gitterkonstanten a = 983,2(2), b = 2119,2(3), c = 2145,1(4) pm, β = 91,97(1)° und vier Molekülen pro Elementarzelle. Die Struktur wurde auf der Grundlage von 2779 beobachteten symmetrieunabhängigen Reflexintensitäten nach der Schweratommethode gelöst und bis zu einem R-Wert von 0,063 (RW = 0,052) verfeinert. Das Ni-Atom als Spirozentrum ist verzerrt tetraedrisch von den vier P-Atomen der beiden zweizähnigen Chelatliganden umgeben. Die sehr ähnlichen Ni-P-Abstände weisen einen Mittelwert von 216(1) pm auf. Der aus der Molekülstruktur von [Ni(dppe)2] berechnete mittlere Öffnungswinkel für den Tolman-Kegel von dppe beträgt 129,8°.
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  • 6
    ISSN: 1436-2449
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Summary An inert non-crystalline cryoprotectant oil was needed as a non-incoherent scattering matrix for neutron studies of solvent containing crystalline materials. This led us to prepare perdeuterated polyethylpropylene (PEP) with a molar mass around 1100 g/mol. On route to this material an improved method for the preparation of isoprene-d8 starting from calcium carbide and acetone-d6 was devised. Subsequent anionic polymerization using t-butyl lithium as initiator resulted in an oligomeric perdeuterated polyisoprene (PI) with an average chain length of approx. 15 monomer units and Mw/Mn: 1.1. This polymer was deuterated with D2 and Pd/C (10%) in cyclohexane to yield the desired perdeutero polymer (PEP-d). The polymer fulfill the important properties that it does not crystallize at low temperature and has a low neutron scattering efficiency.
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  • 7
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 395 (1973), S. 112-118 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Organo Thallium DithiophosphatesSynthesis and properties of the monophenyl- and the diphenylthalliumdithiophosphates are reported and the relative stability of the organothalliumderivatives of the type RnTI[S(S)P(OR′) (OR")]3-n is discussed.
    Notes: Es wird über die Darstellung und die Eigenschaften von Mono-phenyl- und Diphenylthallium -dithiophosphaten berichtet und die relative Stabilität von Organothalliumderivaten des Typs RnTl[S(S)P(OR′) (OR")]3-n is diskutiert.
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  • 8
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Insertion Reactions to the Organothallium (III)-Element BondInsertion reactions to the thallium-element bonds of Me2Tl-NMe2 and Me2TI-OEt with RNCS, PhNCO, CS2. COS, CO2, SO2 and SO3 and the characterization of the reaction products with the chemical and spectroscopic methods are reported.
    Notes: Es wird über Einschiebungsreaktionen in die Thallium-Element-Bindungen von Me2TI-NMe2 bzw. Me2TI-OEt mit RNCS, PhNCO, CS2, COS, CO2, SO2 und SO3 sowie die Charakterisierung der Reaktionsprodukte mit chemischen und spektroskopischen Methoden berichtet.
    Additional Material: 2 Ill.
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  • 9
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: 31P and 195Pt N.M.R. Investigations on Diplatinum (I) Complexes of the Type [Pt2(μ-SPR2)2L2] (L = PR3, PhP(OPh)2, P(OPh)3, CNR)31P-, 195Pt-chemical shifts and 195Pt-31P- resp. 31P-31P-coupling constants of a series of doubly bridged diplatinum(I) complexes are reported. 31P-coordination chemical shifts of the terminal ligands of complexes of type [Pt2(μ-SPR2)2(P′R3′)2] and some of the various coupling constants are strongly influenced by the π-acceptor strength of these ligands. J(195Pt-195Pt) is found to change the sign among the series of complexes investigated. Thermal singlett triplet exitation giving rise to the paramagnetism of these complexes observed by preliminary EPR-measurements and confirmed by EHT-calculations is deduced from the large values of 2J(P-P′) and 3J(P′P′) as well as the unusually high temperature dependence of some coupling constants and other NMR features. The chemical stability of the doubly bridged core, the coordination shifts of the bridging phosphorus atoms and EHT-calculations suggest a view of aromaticity of the [Pt2(μ-SPR2)2](M-M) unit of these complexes.
    Notes: Es werden 31P-, 195Pt-chemische Verschiebungen und 195Pt31P-Kopplungskonstanten einer Reihe von doppelt verbrückten Diplatin(I)-Komplexen mitgeteilt. 31P-koordinationschemische Verschiebungen der ternären Liganden von Komplexen des Typs [Pt2(μ-SPR2)2(P′R3′)2] und verschiedene Kopplungskonstanten werden stark von der π-Akzeptor-Stärke dieser Liganden beeinflußt. J(195P-195Pt) wird innerhalb der Reihe der untersuchten Komplexe mit wechselndem Vorzeichen gefunden. Aus den großen Werten von 2J(Pt-P′) und 3J(P′P′) sowie der ungewöhnlich starken Temperaturabhängigkeit einiger Kopplungskonstanten und anderen NMR-Eigenschaften wird auf Paramagnetismus dieser Komplexe aufgrund thermischer Singlett-Triplett-Anregung geschlossen, der in vorläufigen EPR-Messungen gefunden und durch EHT-Rechnungen gestützt wird. Die chemische Stabilität des doppelt verbrückten Kerns, die koordinationschemischen Verschiebungen der Brückenphosphoratome und EHT-Rechnungen weisen auf Aromatizität der [Pt2(μ-SPR2)2](M-M)-Einheit dieser Komplexe hin.
    Additional Material: 5 Ill.
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  • 10
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Secondary Phosphine Chalcogenides. VII. Synthesis of Bis(tert.-butylphosphino)thane, ButHPCH2CH2PHBut, and 1-tert.-Butylphosphino-2-diphenylphosphinoethane, Ph2PCH2CH2PHBut, as well as their Secondary Phosphine ChalcogenidesThe reaction of Cl2PCH2CH2PCl2 with ButMgCl gives ButClPCH2CH2PClBut which is either hydrolysed to yield ButH(O)PCH2CH2P(O)HBut or reduced to give ButHPCH2CH2PHBut. This phosphine reacts with sulfur or selenium to give ButH(E)PCH2CH2P(E)HBut (E = S, Se).Treatment of Ph2PCH2CH2Cl with LiPHBut results Ph2PCH2CH2PHBut which is oxidized to give Ph2(E)PCH2CH2P(E)HBut (E = O, S, Se). The Ph2P group appears to be oxidized primarily. The compounds obtained are characterized by means of I.R. 1H and 31P-N.M.R. spectroscopy.
    Notes: Durch Reaktion von Cl2PCH2CH2PCl2 mit Bu1MgCl wird ButClPCH2CH2PClBut erhalten, das entweder zu ButH(O)PCH2CH2P(O)HBut hydrolysiert oder zu ButHPCH2CH2PHBut reduziert wird. Dieses PHosphin ergibt mit Schwefel bzw. Selen ButH(E)PCH2CH2P(E) HBut (E = S, Se).Ph2PCH2CH2Cl und LiPHBut setzen sich zu Ph2PCH2CH2PHBt um, das zu Ph2(E)PCH2CH2P(E)HBt (E = O, S, Se) oxidiert wird, wobei primär die PH2P-Gruppe reagiert. Die dargestellten Verbindungen werden mit Hilfe ihrer IR-, 1H- und 31P-Spektren charakterisiert.
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