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  • 1
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 593 (1991), S. 207-216 
    ISSN: 0044-2313
    Keywords: Cesium Diaquatetrafluoro Metallates ; Aluminium ; Chromium ; Manganese ; Iron ; Crystal Structure ; IR Spectra ; Thermochemistry ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Structural Chemistry of Compounds Cs[MF4(H2O)2] (M = Al, Cr, Mn, Fe)The compounds Cs[MF4(H2O)2] (M = Al, Br, Fe) have been prepared and the structures explored by means of X-ray diffraction, in the case of the Al compound on a single crystal. They crystallize isotypic with Rb[VF4(H2O)2] and Cs[MnF4(H2O)2] in space group I2/a, Z = 4 [Cs]AlF4(H2O)2: a = 882.4(3); b = 667.8(1); c = 1 002.4(3) pm; β = 105.14°; R = 0.025 for 1685 reflections. Cs[CrF4(H2O)2]: a = 895.3; b = 669.1; c = 1 014.5; β = 104.40°. Cs[FeF4(H2O)2]: a = 906.6; b = 673.1; c = 1 027.2; β = 104.73°). The [AlF4(H2O)2]- anions with trans aqua ligands are linked via strong H-bonds (O…F 257-251 pm) to form chains which are further connected to a 3-dim. network. This is expressed as well in the i.r. spectra. The thermal decomposition leads, in one step, to the water free tetrafluorometallates.
    Notes: Die Verbindungen Cs[MF4(H2O)2] (M = Al, Cr, Fe) wurden dargestellt und ihre Strukturen röntgenographisch - im Falle der Al-Verbindung an einem Einkristall - untersucht. Sie kristallisieren isotyp zu Rb[VF4(H2O)2] und Cs[MnF4(H2O)2] in Raumgruppe I2/a, Z = 4 [Cs[AlF4(H2O)2]]: a = 882,4(3); b = 667,8(1); c = 1 002,4(3) pm; β = 105,14°; R = 0,025 für 1 685 Reflexe. Cs[CrF4(H2O)2]: a = 895,3; b = 669,1; c = 1 014,5; β = 104,40°. Cs[FeF4(H2O)2]: a = 906,6; b = 673,1; c = 1 027,2; β = 104,73°). Die [AlF4(H2O)2]--Anionen mit transständigen Aqualiganden sind über starke H-Brücken (O…F 257-261 pm) zu dreidimensional vernetzten Ketten miteinander verbunden. Dies kommt auch in den IR-Spektren zum Ausdruck. Die thermische Zersetzung führt einstufig zu den wasserfreien Tetrafluorometallaten.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 0044-2313
    Keywords: Osmium Polysulfido Complex ; Synthesis ; IR Spectrum ; 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 Tetraphenylphosphonium Aqua-bis(tetrasulfido)thionitrosyl Osmate, PPh4[Os(NS)(S4)2(H2O)]PPh4[Os(NS)(S4)2(H2O)] has been prepared as redbrown crystals by reacting PPh4[OsNCl4] with a solution of excess disodium tetrasulfide in dimethylformamide/H2O and characterized by IR spectroscopy and by a crystal structure determination. Space group P21/n, Z = 4, structure solution with 4162 independent reflections, R = 0.059 for reflections with I 〉 2σ(I). Lattice dimensions at -40°C: a = 1138.9(5), b = 1301.4(4), c = 2092.7(7) pm, β = 104.74(3)º. Os—N, Os—O, and Os—S distances are 175.2(12), 219.8(12), and 237.5(4)-239.1(4) pm, respectively. The Os=N=S moiety is approximately linear, with an OsNS angle of 171.2(7)º.
    Notes: PPh4[Os(NS)(S4)2(H2O)] wurde als rotbraune Kristalle durch Reaktion von PPh4[OsNCl4] mit einer Lösung von überschüssigem Dinatriumtetrasulfid in Dimethylformamid/H2O hergestellt und durch das IR-Spektrum und eine Kristallstrukturanalyse charakterisiert. Raumgruppe P21/n, Z = 4, Strukturlösung mit 4162 unabhängigen Reflexen, R = 0,059 für Reflexe mit I 〉 2σ(I). Gitterabmessungen bei -40°C: a = 1138,9(5); b = 1301,4(4); c = 2092,7(7) pm, β = 104.74(3)º. Die Abstände Os—N, Os—O und Os—S betragen 175,2(12), 219,8(12) und 237,5(4) - 239,1(4) pm. Die Os=N=S-Gruppe ist mit einem Bindungswinkel von 171,2(7)º annähernd linear.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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