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  • 1
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 608 (1992), S. 17-22 
    ISSN: 0044-2313
    Keywords: Barium-crownether complex ; octaselenido cadmate ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structure of [Ba(18-Crown-6)(DMF)4][Cd(Se4)2]The title compound has been prepared by the reaction of a DMF-solution of lithium polyselenide with BaSe2 and cadmium acetate in the presence of 18-crown-6, forming black crystals. The compound was characterized by IR spectroscopy and by an X-ray structure determination. Space group P2/a, Z = 4, 5392 observed unique reflections, R = 0.048. Lattice dimensions at -90°C: a = 2021.9(12); b = 1019.8(6); c= 2270.8(14)pm, ß = 106.98(4)°. The structure consists of [Ba(18-crown-6)(DMF)4]2+ ions, in which the barium ions are coordinated by the six oxygen atoms of the crown ether molecule and by four oxygen atoms of the DMF molecules, and of [Cd(Se4)2]2- ions. The cadmium atoms are coordinated by two tetraselenide ions in a chelating fashion.
    Notes: Die Titelverbindung entsteht in Form schwarzer Kristalle bei der Einwirkung einer Lithiumpolyselenidlösung auf Bariumdiselenid und Cadmiumacetat in Dimethylformamid in Gegenwart von 18-Krone-6. Die Verbindung wurde durch das IR-Spektrum und eine röntgenographische Strukturanalyse charakterisiert. Raumgruppe P2/a, Z = 4, 5392 beobachtete unabhängige Reflexe, R = 4,8%. Gitterabmessungen bei -90°C: a = 2021,9(12); b = 1019,8(6); c = 2270,8(14) pm, ß = 106,98(4)°. Die Struktur ist aufgebaut aus [Ba(18-Krone-6)(DMF)4]2+-Ionen, in denen die Bariumionen von den sechs Sauerstoffatomen des Kronenethers und von vier O-Atomen der DMF-Moleküle koordiniert sind, und [Cd(Se4)2]2- -Anionen. In diesen sind die Cadmiumatome von zwei Tetraselenidionen chelatartig umgeben.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 0044-2313
    Keywords: Mixed polyselenido complexes of zinc/tungsten, Mercury/tungsten ; crystal structures ; FIR spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Syntheses and Crystal Structures of the Polyselenido Complexes (PPh4)6[M(Se4)2]2[WSe4] · DMF with M = Zinc and MercuryThe title compounds have been prepared by the reactions of the acetates of zinc and mercury, respectively, with excess (PPh4)2 WSe4 in boiling dimethylformamide, forming black-red single crystals. According to the X-ray structure determinations both compounds crystallize isotypically in the space group 12/a with four formula units per unit cell. (PPh4)6[Zn(Se4)2]2[WSe4] · DMF: a = 2888.1(6), b = 1740.3(2), c = 2893.9(4) pm, β = 90.47(1)°. 3230 observed unique reflections, R = 0.009.(PPh4)6[Hg(Se4)2]2[WSe4] · DMF: a = 2891.8(5), b = 1738.0(4), c = 2920.1(5) pm, β = 90.29(2)°. 2978 observed unique reflections, R = 0.115%.The compounds consist of PPh4+ ions, spirocyclic octaseleno metallates [M(Se4)2]2-, tetrahedral WSe42-ions, and disordered DMF Molecules.
    Notes: Die Titelverbindungen entstehen in Form schwarz-roter Einkristalle beim Erhitzen der Acetate von Zink und Quecksilber mit überschüssigem (PPh4)2 WSe4 in Dimethylformamid-Lösungen. Nach den Röntgenstrukturanalysen kristallisieren die Verbindungen isotyp in der Raumgruppe I2/a mit vier Formeleinheiten pro Elementarzelle. (PPh4)6[Zn(Se4)2]2[WSe4]· DMF: a = 2888,1(6), b = 1740,3(2), c = 2893,9(4) pm, β = 90,47(1)°. 3230 beobachtete unabhängige Reflexe, R = 9,9%.(PPh4)6[Hg(Se4)2]2[WSe4] · DMF: a = 2891,8(5), b = 1738,0(4), c = 2920,1(5) pm, β = 90,29(2)°. 2978 beobachtete unabhängige Reflexe, R = 11,5%.Die Verbindungen bestehen aus PPh4 +-Ionen, spirocyclischen Octaselenometallaten [M(Se4)2]2-, tetraedrischen WSe42- Ionen und eingelagerten, fehlgeordneten DMf-Molekülen.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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