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  • 1
    ISSN: 0044-2313
    Keywords: Pentachloromonocarbonylosmate(III) ; Crystalline Hydrate ; Crystal Structure ; Vibrational Spectra ; Normal Coordinate Analysis ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis, Crystal Structure, Vibrational Spectra, and Normal Coordinate Analysis of K2[OsCl5(CO)] · H2OThe X-ray structure determination of K2[OsCl5(CO)] · H2O (monoclinic, space group P21/c a = 13.600(2), b = 7.122(1), c = 22.186(11) Å, β = 98.66(3)°, Z = 8) revealed two crystallographic independent bat very similar complex anions [OsCl5(CO)]2- with rough C4v point symmetry. Due to the stronger trans influence of the carbonyl group the bond lengths in the Cl—Os—CO axis Os—Cl = 2.449(2), 2.430(2) Å are langer as compared with the octahedron basis Os—Cl = 2.340-2.370 Å. The water of crystallization is coordinated to potassium (K—OH2 = 2.625-2.815 Å). Using the molecular parameters the IR and Raman spectra are assigned by normal coordinate analysis. The valence force constants are fd(CO) = 15.30, fd(OsC) = 3.88, fd(OsCl) = 1.81, fd(OsCl) = 1.36, fd(OH) = 7.65, 7.82, 7.79 mdyn/Å. The strengthening of the Os—C bond by stronger back donation of the OsIII(d5) complex in comparison with the isostructural OsIV (d4) compound is discussed.
    Notes: Die Röntgenstrukturanalyse von K2[OsCl5(CO)] · H2O (monoklin, Raumgruppe P21/c a = 13,600(2), b = 7,122(1), c = 22,186(11) Å, β = 98,66(3)°, Z = 8) hat gezeigt, daß zwei kristallographisch unabhängige aber sehr ähnliche Komplexanionen [OsCl5(CO)]2- mit annähernd C4v-Punktsymmetrie vorliegen. Durch den größeren trans-Einfluß der Carbonylgruppe sind die Bindungsabstände in der Cl—Os—CO Achse Os—Cl = 2,449(2), 2,430(2) Å länger als in der Oktaederbasis: Os—Cl = 2,340-2,370 Å. Das Kristallwasser ist an Kalium koordiniert (K—OH2 = 2,625-2,815 Å). Mit den röntgenographisch bestimmten Molekülparametern lassen sich die IR- und Raman-Spektren durch Normalkoordinatenanalyse zuordnen. Die Valenzkraftkonstanten betragen fd(CO) = 15,30, fd(OsC) = 3,88, fd(OsCl) = 1,81, fd(OsCl) = 1,36, fd(OH) = 7,65, 7,82, 7,79 mdyn/Å. Die Festigung der Os—C-Bindung durch stärkere Rückbindung in dem OsIII(d5)-Komplex im Vergleich zur isostrukturellen OsIV(d4)-Verbindung wird diskutiert.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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