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  • 1
    ISSN: 1520-510X
    Source: ACS Legacy Archives
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 0009-2940
    Keywords: Bis-arene complexes ; Niobium complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Bis(mesitylen)niobium(0), Nbmes2, prepared via the NbCl5/Al/AlCl3/mes system by exaustive reduction in the presence of 1,2-dimethoxyethane or tetrahydrofuran as previously reported, has been studied by X-ray diffraction methods. The sandwich molecule has parallel, substantially planar, aromatic rings, in an eclipsed conformation. Nbmes2 is oxidized to Nbmes2X by reaction with 1,1-dimethyl-4,4′-bipyridinium halides [methylviologen halides, mvX2 (X = Cl, I)]. The reaction of both halo compounds with CO yielded the niobium(I) derivatives [Nbmes2(CO)] [Nb2(μ-X)3(CO)8]. In the case of X = I an IR study at low temperature has shown the presence of intermediate carbonyl compounds, presumably Nbmes2I(CO) and [Nbmes2(CO)]+. The ionic iodide derivative was shown by X-ray diffraction methods to consist of discrete [Nbmes2(CO)]+ cations and [Nb2(μ-I)3(CO)8]- anions. The two mesitylene groups in the cation are bent and in an eclipsed conformation.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
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  • 3
    ISSN: 0044-2313
    Keywords: Phosphaneiminato complexes of Nb, Mo, W ; reactions with NaF ; triphenylaminophosphonium chloride ; triphenyl-difluorophosphorane ; crystal structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Reactions of Phosphaneiminato Complexes of Niobium, Molybdenum, and Tungsten with Sodium Fluoride. The Crystal Structures of [PPh3NH2]Cl and PPh3F2[NbCl4(NPPh3)]2 reacts with excess sodium fluoride and 15-crown-5 in acetonitrile, forming the fluoro complex [Na-15-crown-5][NbF5(NPPh3)] at room temperature. In boiling acetonitrile the solvent takes part in the cleavage of the Nb—N bond of the phosphaneiminato complex, yielding [PPh3NH2]Cl. In corresponding reactions the phosphaneiminato complexes [MoCl4(NPPh3)]2 and [WCl5(NPPh3)] undergo a cleavage of the P—N bond giving PPh3F2 in a good yield. [PPh3NH2]Cl and PPh3F2 are characterized by crystal structure analyses:[PPh3NH2]Cl: Space group Pna21, Z = 4,1796 observed independent reflexions, R = 0.030. Lattice constants at -60°C: a = 1084.7, b = 961.7, c = 1536.5. The compound consists of PPh3NH2+ ions and chloride ions, which link the cations to … HNH … Cl … HNH … Cl chains.PPh3F2: Space group Pbcn, Z = 4,987 observed independent reflexions, R = 0.044. Lattice constants at 20°C: a = 611.41, b = 1664.2, c = 1436.9. This compound has a trigonal bipyramidal structure with the fluorine atoms in the axial positions.
    Notes: Die Reaktion von [NbCl4(NPPh3)]2 mit überschüssigem Natriumfluorid in Acetonitril führt in Gegenwart von 15-Krone-5 in der Kälte zu dem Fluorokomplex [Na-15-Krone-5][NbF5(NPPh3)]. In der Siedehitze findet unter Mitwirkung des Lösungsmittels Spaltung der Nb—N-Bindung des Phosphaniminatokonplexes statt, wobei [PPh3NH2]Cl gebildet wird. Entsprechende Untersuchungen mit den Phosphaniminatokomplexen [MoCl4(NPPh3)]2 und [WCl5(NPPh3)] führen unter Spaltung der P—N-Bindung zu PPh3F2, das in guter Ausbeute erhalten wird. [PPh3NH2]Cl und PPh3F2 haben wir durch Kristallstrukturanalysen charakterisiert.[PPh3NH2]Cl: Raumgruppe Pna21, Z = 4,1796 unabhängige, beobachtete Reflexe, R = 3,0%. Gitterkonstanten bei -60°C: a = 1084,7; b = 961,7; c = 1536,5 pm. Die Verbindung besteht aus PPh3NH2+-Ionen und Chloridionen, die über Wasserstoffbrückenbindungen … HNH … Cl … HNH … Cl die Kationen zu Ketten verknüpfen.PPh3F2: Raumgruppe Pbcn, Z = 4,987 unabhängige, beobachtete Reflexe, R = 4,4%. Gitterkonstanten bei 20°C: a = 611,41; b = 1664,2; c = 1436,9 pm. Die Verbindung hat eine trigonal-bipyramidale Molekülstruktur mit den Fluoratomen in den Axialpositionen.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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  • 4
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 606 (1991), S. 91-96 
    ISSN: 0044-2313
    Keywords: Lithium chloride crown ether complex ; I.R. spectrum ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: [Li(12-Crown-4)]Cl: Crystal Structure and I.R. SpectrumColourless single crystals of [Li(12-crown-4)]Cl were obtained from acetonitrile solutions of LiCl in the presence of 12-crown-4. They were characterized by i. r. spectroscopy as well as by an X-ray structure determination. Space group P4/n, Z = 2, 1 080 observed unique reflections, R = 0.034. Lattice dimensions at -50°C; a = 837.8(5), c = 752.0(2) pm. [Li(12-crown-4)]Cl forms ion pairs with tetragonal symmetry and bond lengths Li—O of 212.8 pm and Li—Cl of 229.0 pm.
    Notes: [Li(12-Krone-4)]Cl wurde aus LiCl-Lösungen in Acetonitril in Gegenwart von 12-Krone-4 in farblosen Einkristallen erhalten, die durch das IR-Spektrum und eine röntgenographische Strukturanalyse charakterisiert werden. Raumgruppe P4/n, Z = 2, 1080 beobachtete unabhängige Reflexe, R = 3,4%. Gitterabmessungen bei -50°C: a = 837,8(5), c = 752,0(2) pm. [Li(12-Krone-4)]Cl bildet Ionenpaare mit tetragonaler Symmetrie und Abständen Li—O von 212,8 pm und Li—Cl von 229,0 pm.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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