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  • Barium caesium undecaphosphide-ammonia (1/11), BaCsP11 · 11 NH3  (1)
  • Phase-transfer catalysis  (1)
  • 1
    Electronic Resource
    Electronic Resource
    Synthesewege zu neuen ionischen Ozoniden (1992)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 125 (1992), S. 1383-1388 
    Details
    ISSN: 0009-2940
    Keywords: Phase-transfer catalysis ; Ozonides, ionic ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Synthetic Routes to New Ionic OzonidesNew synthetic routes to tetraorganylammonium ozonides involving exchange reactions with alkali metal ozonides were investigated. The previously reported reaction between tetraalkylammonium hyperoxides R4N+O2- (R = Me, Et) and alkali metal ozonides in liquid ammonia is severely hampered by the difficult synthesis of these hyperoxides; they are unknown for other quaternary ammonium cations. A similar reaction between the easily accessible chlorides of trialkylbenzylammonium ions and KO3 yields mixed ozonides/chlorides due to some solubility of KCl in liquid ammonia. The new compounds BzlMe3N+ (O3-)0.6Cl-0.4 (3), BzlEt3N+ (O3-)0.8Cl0.2- (4) and Bzl(nBu)3N+(O3-)0.5Cl0.5- (5) were prepared by this route. - The by far superior route to new ozonides utilizes macroreticular cation exchange resins in liquid ammonia. Batch equilibration between an excess of the appropriate ionic form of the resin and CsO3 produced Me3PhN+O3- (6), BzlMe3N+O3- (7), Bzl(nBu)3N+O3- (8), and (nPr)4N+ O3- (9) in almost quantitative yield. Compounds 4, 6, and 7 were studied by single-crystal X-ray analysis; the shortening of the ozonide bond length and the widening of the bond angle in comparison to the alkali metal ozonides as well as the possibility of C-H…O hydrogen bonding are discussed. Thermal stabilities were determined by DTA/TG methods, rapid decomposition starts at 59-79°C for 3, 6, and 7 and at 28-56°C for the remaining new ozonides which contain detachable β-H atoms.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19921250613
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  • 2
    Electronic Resource
    Electronic Resource
    Preparation and crystal structure of barium caesium undecaphosphide-ammonia (1/11) BaCsP11 · 11 NH3Dedicated to Professor Hans-Georg von Schnering on the Occasion of his 65th Birthday (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 1833-1838 
    Details
    ISSN: 0044-2313
    Keywords: Barium caesium undecaphosphide-ammonia (1/11), BaCsP11 · 11 NH3 ; barium nonaammine complex ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Darstellung und Kristallstruktur von Barium-Caesium-Undecaphosphid-Ammoniak (1/11) BaCsP11 · 11 NH3Die neue Verbindung BaCsP11 · 11 NH3 wurde in flüssigem Ammoniak ausgehend von Cs3P11 und einem mit Ba2+ -Ionen beladenen Ionenaustauschmaterial hergestellt. BaCsP11 · 11 NH3 bildet gelbe Kristalle, die sich ab 246 K unter Verlust des Kristallammoniaks zersetzen. Die Kristallstruktur wurde mit Hilfe von Röntgen-Einkristalldiffraktometerdaten bestimmt: P21/a, a = 1599.9(2) pm, b = 1793.9(3) pm, c = 1998.1(7) pm, β = 93.02(4)°, Z = 8, wR2 = 0.118 (R1 = 0.047) für 8969 Strukturfaktoren und 631 variable Parameter. Die Kationen Cs+ sind durch Undecaphosphatrishomocuban-Anionen P113- so koordiniert, daß eindimensional-unendliche Stränge ∞1[CsP11]2- vorliegen, die voneinander durch Ba(NH3)n2+ -Kationen (n = 8 und 9) getrennt sind. Es wird nur ein direkter Ba—P-Kontakt beobachtet.
    Notes: The new compound BaCsP11 · 11 NH3 was prepared in liquid ammonia, using Cs3P11 and a cation exchange resin loaded with Ba2+ cations as starting materials. BaCsP11 · 11 NH3 forms yellow crystals which decompose at 246 K under loss of the ammonia of crystallisation. The crystal structure was determined from single-crystal X-ray diffractometer data: P21/a, a = 1599.9(2) pm, b = 1793.9(3) pm, c = 1998.1(7) pm, β = 93.02(4)°, Z = 8, wR2 = 0.118 (R1 = 0.047) for 8969 structure factors and 631 variable parameters. The Cs+ cations are co-ordinated by undecaphosphatrishomocubane anions P113- in such a way that one-dimensionally infinite chains ∞1[CsP11]2- result which are separated by Ba(NH3)n2+ (n = 8 and 9). Only one Ba—P contact is observed.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19966221106
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    Paper (German National Licenses)
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