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  • 1
    ISSN: 0030-493X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The compounds Pt3(CO)3[P(C6H5)3]4 molecular weight 1717, Pt4(CO)5[P(C6H5)3]4 molecular weight 1968 and Pt5(CO)6[P(C2H5)3]4 molecular weight 1615 are thermally labile and are slowly solvolysed by tetrahydrofuran and acetone. They cannot be analysed by means of electron impact. Field desorption, however, shows the molecular ion and [M—xCO]+· peaks.
    Additional Material: 2 Tab.
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  • 2
    ISSN: 0030-493X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Electron impact spectra of thermolysis products of organic salts heated in the ion source of a mass spectrometer may give rise to organic ions corresponding to the cation of the salt. Field ionization mass spectrometry has been used as a facile method for detemining whether such an ion is due to ionization of the corresponding radical present in the gas phase, or to an electron impact induced fragmentation of a reaction product of higher mass. By comparison of the electron impact and field ionization spectra of a series of N-methyl pyridinium, tropylium and 1,2-dithiolylium salts it has been found possible to identify the radicals formed thermolytically, when present.
    Additional Material: 4 Ill.
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  • 3
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Ni(PF3)4 (1) tauscht mit Lithiumorganylen und Grignard-Reagentien Fluor gegen Organyl-Gruppen aus, wobei die Komplexe (10-32) Ni(PF3)4-n(PF2R)n (n = 1, 2 und 3), Ni(PF3)3(PFR2), Ni(PF3)2(PF2R)(PFR2) und Ni(PF3)3(PR3) (R = organ. Rest) gebildet werden. Für den Reaktionsablauf wird ein Vierzentren-Synchron-Mechanismus vorgeschlagen.Fluorine Exchange in Trifluorophosphane Metal Complexes. X. Reactions of Tetrakis(trifluorophosphane)nickel(0) with Metal OrganylsThe fluorine atoms in Ni(PF3)4 (1) can be partially substituted by organyl groups yielding the complexes (10-32) Ni(PF3)4-n(PF2R)n (n = 1, 2 and 3), Ni(PF3)3(PFR2), Ni(PF3)2(PF2R)(PFR2) and Ni(PF3)3(PR3) (R = organyl group). The mechanism of these peripheric reactions is discussed by assuming a four centered type intermediate.
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  • 4
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 490 (1982), S. 111-120 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: News on Pentafluoro Metallates(III), SrNiF5, BaNiF5, BaCoF5, and CdCoF5Samples of BaNiF5 and for the first time SrNiF5 have been prepared by pressure fluorination (monel-autoclaves, pF2 = 50 bar, 400°C, 48 h and pF2 = 20-30 bar, 420 ± 30°C, 4 d, respectively). On the other side BaCoF5 and CdCoF5 are obtained by heating in a diluted stream of F2.Crystal data are BaNiF5: light grey-violet, orthorhombic, a = 987.3(1), b = 547.19(6), c = 743.87(8) pm; SrNiF5; dark-brown, BaGaF5-type of structure, a = 1 326.5(2), b = 544.04(6), c = 492.69(5) pm; BaCoF5: light blue, orthorhombic, a = 1 392.2(2), b = 562.01(7), c = 496.50(6) pm; CdCoF5: light blue, a = 878.7(2), b = 641.01(8), c = 749.5(2) pm, β = 115.27(2)°, CaCrF5-type of structure.The Madelung Part of Lattice Energy, MAPLE, of SrNiF5 and CdCoF5 is discussed.
    Notes: Durch Fluorierung unter erhöhtem Druck (Monel-Autoklav, pF2 = 50 bar, 400°C, 48 h) wurden hellgrauviolette Proben von BaNiF5 (orthorhombisch, a = 9,873(1); b = 5,4719(6); c = 7,4387(8) Å) sowie erstmals braunes (Monel-Autoklav, pF2 = 20-30 bar, 420 ± 30°C, 4 d) SrNiF5 (BaGaF5-Typ, a = 13,265(2); b = 5,4404(6); c = 4,9269(5) Å) erhalten.Dagegen entstehen hellblaue Pulver von BaCoF5 (orthorhombisch; a = 13,922(2); b = 5,6201(7); c = 4,9650(6) Å) und CdCoF5 (CaCrF5-Typ; a = 8,787(2); b = 6,4101(8); c = 7,495(2) Å, β = 115,27(2)°) bereits im verdünnten Fluorstrom.Der Madelunganteil der Gitterenergie, MAPLE, von SrNiF5 und CdCoF5 wurde diskutiert.
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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: On Li2NiF5 and Na2NiF6.For the first time pure samples of Na2[NiF6] (carmine red; monoklinic, a = 7.564, b = 5.686, c = 5.378 Å, β = 92.28°; Z = 2) have been obtained by pressure fluorination (monel-autoklavs, pF2 = 300 bar, 300°C, 18h) and indexed.Similarly (monel-autoklavs, pF2 = 300 bar, 300°C, 10h) samples of Li2NiF5 (violet; monoclinic, a = 9.788, b = 4.886, c = 9.966 Å; β = 135.56°; Z = 4) have been prepared.
    Notes: Durch Fluorierung unter erhöhtem Druck (Monel-Autoklav, PF2 = 300 bar, 300°C, 18 h) konnten erstmals reine Proben von Na2[NiF6] (karminrot; monoklin, a = 7,564, b = 5,686, c = 5,378 Å; β = 92,28°; Z = 2) dargestellt und indiziert werden.Ebenfalls unter erhöhtem Fluordruck (Monel-Autoklav, pF2 = 300 bar, 300°C, 10h) wurden violette Proben von Li2NiF5 (monoklin, a = 9,788, b = 4,886, c = 9,966 Å; β = 135,56°; Z = 4) erhalten.
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  • 6
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Contributions on the Thermal Behaviour of Sulfates. VI. On the Chemical Transport of CuSO4, Cu2OSO4, and CuOA powder of anhydrous CuSO4 can be prepared by heating CuSO4 · 5 H2O in air or in an argon atmosphere. In the same way it is possible to get a powder of Cu2OSO4. But up to now, it was difficult to get crystals of CuSO4 and there was no method known to synthesize crystals of Cu2OSO4. Investigations concerning chemical transport reactions of anhydrous heavy metal sulfates showed, that it is possible to get well formed crystals of CuSO4 and Cu2OSO4 by deposition from a vapour phase. As transport agents for CuSO4, Cl2 and HgCl2 are especially suitable. Less appropriate are HCl, NH4Cl, and I2.The chemical vapor deposition of Cu2OSO4 proceeds well with HgCl2. In course of these investigations we recognized, that for CuO in addition to the well approved transport agents also Cl2, HgCl2 or I2 (NH4Cl less suitable) can successfully be used.
    Notes: Wasserfreies CuSO4 ist in Pulverform durch thermischen Abbau der Hydrate leicht zugänglich, pulverförmiges Cu2OSO4 läßt sich dementsprechend aus CuSO4 darstellen. Kristalle waren dagegen bisher von CuSO4 nur sehr schwierig und von Cu2OSO4 noch nicht synthetisch zu gewinnen. Wie sich im Rahmen einer Untersuchung zum chemischen Transport wasserfreier Schwermetallsulfate zeigte, sind gut ausgebildete Kristalle von CuSO4 und Cu2OSO4 durch Abscheidung aus der Gasphase zugänglich. Als Transportmittel für CuSO4 sind besonders Cl2 und HgCl2 geeignet, weniger brauchbar sind HCl, NH4Cl oder I2. Das Oxidsulfat ist mit HgCl2 und NH4Cl, weniger gut mit I2 zu transportieren. Dabei fanden wir, daß für CuO außer den dafür bereits erprobten Transportmitteln auch Cl2, HgCl2 und I2 (NH4Cl weniger gut) verwendbar sind.
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  • 7
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Structural Chemistry of Phosphorus Containing Chains and Rings. 11. Crystal and Molecular Structures of the Two Stereoisomers of Tetraphospha-silaspiro[2.2]pentane (PBut)2Si(PBut)2The spirocyclic compound 1,2,4,5-tetra-tert-butyl-1,2,4,5-tetraphospha-3-silaspiro[2.2]pentane exists in tow diastereomers of point symmetry 4 and 2. The isomer with symmetry 4 even in the solid crystallizes tetragonally in I41/a with a = 1247.0, c = 1505.5 pm and Z = 4. The isomer of fairly exact symmetry 2 crystallizes triclinically in P1 with a = 612.8, b = 996.3, c = 1017.2 pm, α = 75.63, β = 72.38, γ = 88.71° and Z = 1. In this disordered structure the surroundings of Si is slightly distorted due to the influence of the substituents. The (average) bond lengths are (4, 2): d(Si—P) = 220.09(9), 221.5(5); d(P—P) = 225.5(2), 224.2(5); d(P—C) = 189.4(3), 190(2); d(C—C) = 151.4(4), 152(3) pm. The geometry of the substituents in both isomers is quite normal.
    Notes: Die Spiroverbindung 1,2,4,5-Tetra-tert-butyl-1,2,4,5-tetraphospha-3-silaspiro[2.2]pentan liegt in zwei Diastereomeren der Punktsymmetrie 4 und 2 vor. Das Isomer der auch im Festkörper exakten Symmetrie 4 kristallisiert tetragonal in der Raumgruppe I41/a mit a = 1247,0, c = 1505,5 pm und Z = 4. Das sterisch weniger günstige Isomer der im Festkörper nicht streng erfüllten Symmetrie 2 kristallisiert triklin in der Raumgruppe P1 mit a = 612,8, b = 996,3, c = 1017,2 pm, α = 75.63, β = 72,38, γ = 88,71° und Z = 1. In dieser nur fehlgeordnet beschreibbaren Struktur wird die Umgebung des Si durch Substituenteneinflüsse etwas verzerrt. Die (mittleren) Bindungslängen betragen (4, 2): d(Si—P) = 220,09(9), 221,5(5); d(P—P) = 225,5(2), 224,2(5); d(P—C) = 189,4(3), 190(2); d(C—C) = 151,4(4), 152(3) pm. Die Geometrie der Substituenten ist in beiden Isomeren normal.
    Additional Material: 3 Ill.
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  • 8
    ISSN: 0021-8383
    Keywords: Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: INDO Calculation of 15N-13C Coupling Constants in Simple Cyanines and Merocyanines
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  • 9
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 489 (1982), S. 7-10 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Dimorphism of BaNiF6By pressure fluorination synthesis bright carmine red samples of Ba[NiF6] (monoclinic, a = 9.465; b = 4.950; c = 9.516 Å, β = 103.4°; Z = 4) are obtained. The trigonal modification (BaGeF6-type of structure, a = 7.268; c = 6.981 Å, Z = 3) is formed under static pressure (300°C, 50 kbar) only. The bond length Ni—F = 1.78 Å is discussed by means of the Madelung Part of the Lattice Energy, MAPLE. The magnetic behaviour is studied.
    Notes: Bei der Fluorierung unter erhöhtem Druck entstehen karminrote Proben von Ba[NiF6](monoklin, a = 9.465; b = 4,950; c = 9,615 Å; β =103,4°; Z = 4) Erst unter statischem Druck (300°C, 50 kbar) entsteht die trigonale Form (BaGeF6-Typ, a = 7,268; c = 6,981 Å, Z = 3). Die Bindungslänge Ni—F = 1,78 Å wurde über MAPLE-Rechnungen bestimmt. Das magnetische Verhalten wird diskutiert.
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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: Contributions to the Chemistry of Phosphorus. 115. Synthesis and Properties of the Tetraphospha-silaspiro[2.2] pentane (PBut)2Si(PBut)2The first spirocyclic phosphorus-silicon three-membered ring compound, 1,2,4,5-tetra-tert-butyl-1,2,4,5-tetraphospha-3-silaspiro[2.2]pentane, (PBut)2Si(PBut)2 (1), has been synthesized by cyclocondensation of K(But)P—P(But)K with silicon tetrachloride in the molar ratio of 2:0.9. It was characterized by elemental analysis, cryoscopic molecular weight determination and its mass, magnetic resonance and vibrational spectra. 1 is formed as a mixture of two diastereomers 1a and 1b. These differ in the relative arrangement of the trans-oriented organyl substituents at the two three-membered rings; both isomers could be obtained in a pure state. The sterically less favoured isomer 1b rearranges into the comparatively more stable isomer 1a.
    Notes: Die erste spirocyclische Phosphor-Silicium-Dreiringverbindung, das 1,2,4,5-Tetra-tert-butyl-1,2,4,5-tetraphospha-3-silaspiro[2.2]pentan, (PBut)2Si(PBut)2 (1), wurde durch Cyclokondensation von K(But)P—P(But)K mit Siliciumtetrachlorid im Molverhältnis 2:0,9 synthetisiert. Die Charakterisierung erfolgte durch Elementaranalyse, kryoskopische Molmasse-Bestimmung, Massen-, Kernresonanz- und Molekülschwingungsspektren. 1 entsteht als Gemisch von zwei Diastereomeren 1a und 1b, die sich in der Anordnung der jeweils trans-ständigen Organylgruppen beider Dreiringe zueinander unterscheiden; beide Isomere konnten rein erhalten werden. Das sterisch ungünstigere Isomer 1 b lagert sich in das vergleichsweise beständigere Isomer 1 a um.
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