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  • 1990-1994  (88)
  • Inorganic Chemistry  (83)
  • Analytical Chemistry and Spectroscopy  (5)
  • 1
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 596 (1991), S. 89-92 
    ISSN: 0044-2313
    Keywords: Calcium oxychloride ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: An Oxychloride of Calcium: Ca4OCl6Ca4OCl6 (hexagonal, P63mc, Z = 2), a = 905.8(3), c = 686.3(4) pm, (R = 0.031) crystallizes as colourless needles from reducing melts (CaCl2, Ca) that contain small amounts of „oxygen“. It contains „isolated“ tetrahedral units [Ca4O] and is isotypic with e.g., Ba4OCl6, Yb4OCl6 and K6HgS4. Ca4OCl6 does not form in the dehydration process of, for example, CaCl2 · 6 H2O.
    Notes: Ca4OCl6 (hexagonal, P63mc, Z = 2, a = 905.8(3)); c = 686.3(4) pm, (R = 0,031) kristallisiert in Form farbloser Nadeln aus „reduzierenden Schmelzen“ (CaCl2, Ca), die wenig „Sauerstoff“ enthalten. Es enthält „isolierte“ tetraedrische [Ca4O]-Einheiten und ist isotyp mit z. B. Ba4OCl6, Yb4OCl6 oder K6HgS4. Ca4OCl6 entsteht nicht beim Entwässern von z. B. CaCl2 · 6 H2O.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
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  • 2
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 16 (1993), S. 491-494 
    ISSN: 0935-6304
    Keywords: Supercritical fluid extraction ; Polynuclear aromatic hydrocarbons ; Liquid/solid traps ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Polynuclear aromatic hydrocarbons (PAHs) are recovered from a soil with a high carbon content (ca. 50%) with supercritical fluid extraction (SFE) as well as with conventional Soxhlet extraction. The influence of temperature and modifier volume on SFE efficiency and the effect of a combined liquid/solid trap for analyte collection are investigated in this study. Such traps, which make analyte collection and clean-up possible in one step, are compared with conventional analyte collection in pure organic solvents. A comparison between reproducibility and efficiency of SFE and Soxhlet extraction is presented.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 15 (1992), S. 637-640 
    ISSN: 0935-6304
    Keywords: Capillary GC ; On-column injection ; Plasma samples ; Retinoid analysis ; Acitretin isomers ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The capillary gas chromatographic (CGC) analysis of the der-matological drug trans-acitretin (NeotigasonR) and its cis metabolite is described. Separation of the methyl ester derivatives can be achieved on a 90% biscyanopropylsiloxane phase. The importance of using cold on-column injection and short, thin film capillary columns is discussed. For patients treated with the prodrug of acitretin, etretinate (TigasonR), i.e. the ethyl ester of Neotigason, three compounds have to be separated. Selectivity tuning is required for successful CGC separation. An alternative can be found in the selectivity of ion monitoring mass spectroscopy. Analysis of plasma samples involves liquid-liquid extraction, a derivatization step, and HPLC purification.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
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  • 4
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The intact ion yields of phosphotyrosine, phosphothreonine and mono- and diphosphoserine residue-containing peptides have been compared with the non-phosphorylated sequences using plasma desorption mass spectrometry. Equimolar mixtures of the phosphorylated (MP) and non-phosphorylated peptides (M) were also analysed. The positive mass spectra of these mixtures show a higher intensity of the [M + H]+ compared with the [MP + H]+. In the negative mass spectrum, the bias towards the [M - H]- compared with the [MP - H]- was reduced, but the spectra generally did not accurately reflect the stoichiometry.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
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  • 5
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 27 (1992), S. 1148-1150 
    ISSN: 0030-493X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
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  • 6
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 582 (1990), S. 128-130 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zur Struktur von In5Br7Die Kristallstruktur von In5Br7, die in der Raumgruppe Ce (monoklin, a = 18,688(2); b = 18,602(2); c = 19,217(2) Å; β = 104,19(1)°; Z = 16) verfeinert wurde, muß richtig in der Raumgruppe C2/c beschrieben werden. Revidierte Lageparameter, der Madelunganteil der Gitterenergie, MAPLE, und einige wichtige Abstände werden angegeben.
    Notes: The crystal structure of In5Br7, which was originally described and refined in space group Cc (monoclinic: a = 18.688(2), b = 18.602(2), c = 19.217(2) Å, β = 104.19(1)°, Z = 16), is correctly described in space group C2/c. Revised coordinates, electrostatic parts of the lattice energy (MAPLE), and some important distances are given.
    Additional Material: 3 Tab.
    Type of Medium: Electronic Resource
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  • 7
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 582 (1990), S. 143-150 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Structure and Electrical Conductivity of Ag3YCl6The reaction of YCl3 with an AgCl single crystal in a sandwich diffusion couple (365°C, 140 h) leads to a product layer of single crystalline Ag3YCl6. Single crystals of low-temperature Ag3YCl6-I transform to high-temperature Ag3YCl6-II at 350°C. Ag3YCl6-I (a = 686.69 pm, c = 1830.5 pm, trigonal, R3, Z = 3) is isostructural with Na3GdCl6-I. The compound shows structural disorder with two Ag+-ions occupying statistically half of four octahedral interstices. The specific electrical conductivity of Ag3YCl6 was investigated from room temperature up to the melting point (T = 413°C). The transition from low to high-temperature Ag3YCl6 is accompanied by a sharp increase of the conductivity.
    Notes: Polykristallines YCl3 reagiert mit einem Einkristall von AgCl in Sandwich-Anordnung (365°C, 140 h) an der Kontaktfläche zu einer Produktschicht aus vorwiegend einkristallinem Ag3YCl6. Die daraus isolierten Einkristalle der Tieftemperaturform (Ag3YCl6-I) wandeln sich bei 350°C in eine Hochtemperaturform (Ag3YCl6-II) um. Die Kristallstruktur von Ag3YCl6 I (a = 686,69 pm, c = 1 830,5 pm, trigonal, R3, Z = 3) entspricht der des Na3GdCl6-I. Es liegt eine strukturelle Fehlordnung vor, wobei zwei Ag+-Ionen vier Oktaederlücken statistisch jeweils zur Hälfte besetzen. Die spezifische elektrische Leitfähigkeit von Ag3YCl6 wurde von Raumtemperatur bis oberhalb des Schmelzpunktes (T = 413°C) untersucht. Die Umwandlung der Tiefin die Hochtemperaturform ist von einem sprunghaften Anstieg der Leitfähigkeit begleitet.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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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: Complex Cation [(AnH)3(H2O)2]3+ in Trianilinium-tri-μ-chloro-nonachloro-trirhenate(III)-dihydrate, (AnH)3[Re3(μ-Cl3)Cl9] · 2 H2ODark red single crystals of trianilinium-tri-μ-chloro-nonachloro-trirhenate(III)-dihydrate grow from hydrochloric acid solutions of “ReCl3 · 2 H2O” and anilinium hydrochloride. An important feature of the crystal structure (monoclinic, P21/a, Z = 4, a = 1595.98(12), b = 1594.53(11), c = 1319.65 (9) pm, β = 100.20(1)°, Vm = 497.68(1) cm3 mol-1) are complex cations of the composition [(AnH)3(H2O)2]3+. The N—O- and O—O-distances in the hydrogen bonded cation [(AnH)3(H2O)2]3+ are 281 to 289 pm and 287, respectively. The cationic layers build up corrugated layers parallel (010) and leave two channels in the [010] direction per unit cell into which the anionic clusters, [Re3Cl12]3-, are embedded.
    Notes: Dunkelrote Einkristalle von Trianilinium-tri-μ-chloro-nonachloro-tri-rhenat(III)-dihydrat erhält man aus salzsauren Lösungen von „ReCl3 · 2 H2O“ und Aniliniumhydrochlorid. In der Kristallstruktur (monoklin, P21/a, Z = 4, a = 1595,98(12), b = 1594,53(11), c = 1319,65(9) pm, β = 100,20(1)°, Vm = 497,68(1) cm3 mol-1) sind drei Aniliniumkationen und zwei Wassermoleküle über Wasserstoff-Brückenbindungen zu einem komplexen Kation [(AnH)3(H2O)2]3+ verbunden. Innerhalb dieser Baugruppe findet man N—O-Bindungsabstände zwischen 281 und 289 pm sowie einen O—O-Abstand von 287 pm. Die komplexen Kationen [(AnH)3(H2O)2]3+ sind parallel (010) zu gewellten Schichten angeordnet, die je Elementarzelle zwei Kanäle in Richtung [010] freilassen, in die die Anionen [Re3Cl12]3- eingebettet sind.
    Additional Material: 3 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: Synthesis and Crystal Structure of Praseodymium(III)-monoacetatohexaaquo-dichloridemonohydrate, [Pr(CH3COO)(H2O)6]Cl2 · H2OSingle crystals of [Pr(CH3COO)(H2O)6]Cl2 · H2O (pale green) may be obtained from a solution of PrCl3 · 7 H2O in aqueous acetic acid by isothermic evaporation at room temperature. [Pr(CH3COO)(H2O)6]Cl2 · H2O crystallizes with the triclinic system, space group P1 (No. 2); a = 872.27(9) pm, b = 933.02(8) pm, c = 961.75(9) pm; α = 105.238(9)°, β = 107.913(9)°, γ = 110.568(8)°; R = 0.023, Rw = 0.022 (Z = 2). Pr3+ is nine-coordinated by O2- of six water molecules, one bidentate acetate group, and the bridging oxygen from another (formally monodentate) acetate anion. Centrosymmetric dimers {[Pr(CH3COO)(H2O)6]2}4+ are thus formed, held together by four “lone-some” Cl- anions and two “zeolithic” water molecules per dimer. The chloride ions are surrounded by five (Cl1) and six (Cl2) aquo ligands, respectively. The “zeolithic” water molecule (O9z) has four aquo ligands and two chloride ions (Cl1 and Cl2) as nearest neighbours.
    Notes: [Pr(CH3COO)(H2O)6]Cl2 · H2O wird in Form von blaßgrünen Einkristallen durch Eindunsten wäßriger, essigsaurer Lösungen von PrCl3 · 7 H2O erhalten. Die Verbindung kristallisiert triklin (Z = 2), Raumgruppe P1 (Nr. 2); a = 872,27(9) pm; b = 933,02(8) pm; c = 961,75(9) pm; α = 105,238(9)°; β = 107,913(9)°; γ = 110,568(8)°; R = 0,023; Rw = 0,022. Pr3+ ist von insgesamt neun Sauerstoffatomen umgeben: Sechs gehören zu „Hydratwasser“-Molekülen, zwei zu einer chelatartig angreifenden, das neunte zu einer einzähnig koordinierenden Acetatgruppe. Durch Verbrückung über Acetationen entstehen zentrosymmetrische Dimere {[Pr(CH3COO)(H2O)6]2}4+, die durch vier „einsame“ Cl--Ionen und zwei weitere Wassermoleküle pro Dimer zusammengehalten werden. Die Chloridionen sind von fünf (Cl1) bzw. sechs (Cl2) Wasserliganden umgeben, das „zeolithische“ Wasser (O9z) hat vier Wassermoleküle und zwei Chloridionen (Cl1 und Cl2) als nächste Nachbarn.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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  • 10
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 589 (1990), S. 96-100 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Addition and Substitution of Sodium to/into Cerium(III) Chloride: Na0.38(Na0.19Ce0.81)Cl3The action of sodium on CeCl3 (sealed tantalum ampoule, 750°C, 7 d) yields single crystals of the composition Na0,38(2)(Na0.193(3)Ce0.808(3))Cl3 (hexagonal, P63/m, Z = 2; a = 757.07(4); c = 431.56(3) pm, single-crystal data). The crystal structure may be viewed at as a substitution (Na0,19Ce0,81) plus addition (Na0,38) variant of CeCl3 (UCl3 type of structure).
    Notes: Bei der Einwirkung von Natrium auf CeCl3 (verschweißte Ta-Ampulle, 750°C, 7 d) erhält man Einkristalle der Zusammensetzung Na0,38(2)(Na0,193(3)Ce0,808(3))Cl3 (hexagonal, P63/m, Z = 2; a = 757,07(4); c = 431,56(3) pm, Einkristalldaten). Es liegt eine Substitutions-(Na0,19Ce0,81) und Additionsvariante (Na0,38) des CeCl3 (UCl3-Typ) vor.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
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