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  • Articles: DFG German National Licenses  (7)
  • 1995-1999  (7)
  • preparation  (7)
  • 1
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 201-206 
    ISSN: 0044-2313
    Keywords: Ternary oxides ; anionic gold ; Cs3AuO ; Rb3AuO ; K3AuO ; preparation ; single-crystal structure determination ; analysis of molar volumes ; electrical conductivity ; magnetic properties ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Ternary Oxides containing Anionic GoldThe preparation and crystal structure of the novel ternary oxides M3AuO (M = Cs, Rb, K) containing anionic gold is reported. Cs3AuO (a = 7.830(1) Å, c = 7.060(1) Å) crystallizes as a hexagonal, Rb3AuO (a = 5.501(1) Å) and K3AuO (a = 5.240(1) Å) as a cubic anti perovskite. Concerning to the ionic description (M+)3Au-O2- in Cs3AuO gold exists as an anion. In Rb3AuO and K3AuO the anionic character of gold decreases respectively. The analysis of bond length and molar volumes gives support to this view, as well as investigations of conductivity and magnetic properties do.
    Notes: Über die Darstellung und Kristallstrukturen der neuen ternären Oxide M3AuO (M = Cs, Rb, K) mit anionischem Gold wird berichtet. Cs3AuO (a = 7,830(1) Å, c = 7,060(1) Å) kristallisiert als hexagonaler, Rb3AuO (a = 5,501(1) Å) und K3AuO (a = 5,240(1) Å) als kubischer anti-Perowskit. Gemäß der Formulierung (M+)3Au-O2- liegt Gold in Cs3AuO als Anion vor. In den Verbindungen der leichteren Alkalimetalle nimmt der anionische Charakter von Gold sukzessiv ab. Die Analyse der Bindungslängen und Molvolumina belegt diese Sichtweise, ebenso die durchgeführten Leitfähigkeitsuntersuchungen und magnetischen Messungen.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
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  • 2
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 1901-1906 
    ISSN: 0044-2313
    Keywords: Tetrahydrogen mesoperiodate ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Li2H4I2O10, the First TetrahydrogendimesoperiodateLi2H4I2O10 has been obtained as an intermediate during the dehydration of LiH4IO6 · H2O to LiIO4, for the first time. According to the results of an X-ray structure determination (monoclinic, P21/n, a = 533.98(4), b = 471.85(4), c = 1431.48(10) pm, β = 91.614(7)°, Z = 2, 726 diffractometer data, R = 0.056), Li2H4I2O10 contains the previously unknown tetrahydrogendimesoperiodate ion H4I2O102-, consisting of two edge-shared IO6 octahedra. They are connected with LiO6 octahedra via common edges and vertices. The crystals are non-merohedrally twinned along (100).
    Notes: Li2H4I2O10 wurde als Zwischenstufe während der Entwässerung von LiH4IO6 · H2O zu LiIO4 erstmals erhalten. Nach der Röntgenstrukturanalyse (monoklin, P21/n, a = 533,98(4), b = 471,85(4), c = 1431,48(10) pm, β = 91,614(7)°, Z = 2, 726 unabhängige Reflexe, R = 0,056) liegt das bisher unbekannte Tetrahydrogendimesoperiodatanion H4I2O102- in Form zweier kantenverknüpfter IO6-Oktaeder vor, die ihrerseits mit LiO6-Oktaedern kanten- und eckenverknüpft sind. Die Kristalle sind systematisch verzwillingt. Es handelt sich um monokline Ebenenzwillinge nach (100).
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1803-1809 
    ISSN: 0044-2313
    Keywords: Hyponitrites ; cis-Na2N2O2 ; preparation ; properties ; crystal structure ; vibrational spectra ; 15N-MAS-NMR spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: To the Knowledge of cis-Sodium HyponitriteSurprisingly, cis-sodium hyponitrite can be prepared by reacting gaseous N2O and solid Na2O. For the first time, the structure of a simple salt of cis hyponitrous acid has been determinated unambigously. According to an abinitio structure determination based on powder data, cis-Na2N2O2 crystallizes monoclinic (P21/c, a = 5.107(1); b = 9.211(1); c = 6.159(1) Å; β = 97.91(1)°; Z = 4). Results of spectroscopic investigations (vibrational spectroscopy, 15N-MAS-NMR) agree with the symmetry of the cis-N2O22- anion as it has been proved by the crystal structure. Consider able differences regarding some chemical and physical properties have been observed for samples of cis-Na2N2O2 synthesized via different routes.
    Notes: Durch Gas-Festkörper-Reaktion von N2O und Na2O läßt sich überraschend cis-Natriumhyponitrit darstellen. Auf der Basis der so erhaltenen reinen, gut kristallisierten Präparate gelang erstmals die eindeutige strukturelle Charakterisierung eines einfachen Salzes der cis-Hyposalpetrigen Säure. Gemäß der voraussetzungsfrei anhand von Pulverdaten durchgeführten Strukturbestimmung kristallisiert cis-Na2N2O2 monoklin (P21/c, a = 5,107(1); b = 9,211(1); c = 6,159(1) Å; β = 97,91(1)°; Z = 4). Die Resultate der spektroskopischen Untersuchungen (Schwingungsspektroskopie, 15N-MAS-NMR) stehen im Einklang mit der durch die Kristallstrukturanalyse ermittelten Symmetrie des cis-N2O22--Anions. Präparate von cis-Na2N2O2, die auf verschiedenen Synthesewegen dargestellt wurden, zeigen auffallende Unterschiede in einigen chemischen und physikalischen Eigenschaften.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
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  • 4
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 431-434 
    ISSN: 0044-2313
    Keywords: Ionic ozonides ; preparation ; P(CH3)4O3 ; As(CH3)4O3 ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Knowledge of the New Ionic Ozonides P(CH3)4O3 and As(CH3)4O3P(CH3)4O3 and As(CH3)4O3 were prepared via ion exchange in liquid ammonia and characterized by X-ray-powder, IR, MS and DTA techniques. P(CH3)4O3 and As(CH3)4O3 are isotypic and have a wurtzite-like arrangement of ions with rotationally disordered O3-. (Powder data: P63mc; P(CH3)4O3: a = 687.8(2), c = 964.6(3) pm; As(CH3)4O3: a = 708.6(1), c = 991.0(3) pm). As(CH3)4O3 shows a displacive phase transition at -135°C. The low temperature phase is orthorhombic (a = 715.8(7), b = 1 209(1), c = 943.3(1) pm).
    Notes: P(CH3)4O3 und As(CH3)4O3 wurden mittels Ionenaustausch in fl. NH3 erstmals dargestellt und mit Röntgenpulvermethoden, IR-Spektroskopie, MS und DTA charakterisiert. P(CH3)4O3 und As(CH3)4O3 sind isotyp und bilden eine Ionenpackung im Wurtzit-Typ mit fehlgeordnetem O3-. (Röntgenpulverdaten: P63mc; P(CH3)4O3: a = 687,8(2), c = 964,6(3) pm; As(CH3)4O3: a = 708,6(1), c = 991,0(3) pm). As(CH3)4O3 zeigt bei - 135°C eine displazive Phasenumwandlung. Die Tieftemperaturphase hat orthorhombische Metrik (a = 715,8(7), b = 1 209(1), c = 943,3(1) pm).
    Additional Material: 2 Tab.
    Type of Medium: Electronic Resource
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  • 5
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 484-487 
    ISSN: 0044-2313
    Keywords: Lithiummetaperiodate ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal Structure of Lithiummetaperiodate, LiIO4For the first time single crystals of LiIO4 were obtained. According to the results of an X-ray structure determination (monoclinic, P21/n; a = 525.5(3), b = 851.1(4), c = 796.9(5) pm, β = 104.21(3)°; Z = 4; 2 148 diffractometer data, R = 0.024) the coordination by oxygen is tetrahedral for iodine and strongly distorted trigonal bipyramidal for lithium. Two lithium-oxygen-polyhedra are connected via a common edge. LiIO4 crystallises isostructural to LiAlH4. The structure is discussed and compared to those of other metaperiodates and tetrahydridoaluminates.
    Notes: Erstmals wurden Einkristalle von LiIO4 erhalten. Nach der Röntgenstrukturanalyse (monoklin, P21/n; a = 525,5(3), b = 851,1(4), c = 796,9(5) pm, β = 104,21(3)°; Z = 4; 2 148 unabhängige Reflexe, R = 0,024) wird Iod tetraedrisch und Lithium stark verzerrt trigonal-bipyramidal von Sauerstoff koordiniert. Dabei sind jeweils zwei Lithium-Sauerstoff-Polyeder miteinander kantenverknüpft. Es besteht Isotypie zu LiAlH4. Die Struktur wird diskutiert und mit denen anderer Metaperiodate und Tetrahydridoaluminate verglichen.
    Additional Material: 1 Ill.
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  • 6
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 689-693 
    ISSN: 0044-2313
    Keywords: Fullerenes ; endohedral metallofullerenes ; preparation ; thermodynamics of formation ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Formation of Fullerenes and Endohedral Metallofullerenes: Preparation in a Radiofrequency FurnaceA thermodynamic analysis of the reaction of formation is presented for C60. The alternative route for the preparation of fullerenes by evaporating carbon in a RF-furnace is described. This process is characterized by its broad variability and by comparatively mild conditions which, in addition, may be measured and controlled rather precisely. Thus, it offers favorite facilities for the production of soots with high contents of fullerenes and endohedral fullerenes. So far, LaC82 could be extracted using toluene.
    Notes: Eine thermodynamische Analyse der Bildungsreaktion von C60 wird gegeben und die Darstellung von Fullerenen im Hochfrequenzofen beschrieben. Dieses neue Verfahren zeichnet sich durch eine hohe Variabilität und vergleichsweise schonende Bedingungen aus, die gut meß- und kontrollierbar sind. Es bietet daher günstige Voraussetzungen zur Herstellung von Rußen mit gesteigerten Anteilen höherer Fullerene und, im Falle von Coverdampfungen, endohedraler Metallofullerene. Bisher konnte in Toluolextrakten LaC82 nachgewiesen werden.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
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  • 7
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1055-1060 
    ISSN: 0044-2313
    Keywords: Iodyldisulfate ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The First Crystal Structure Analysis of an Iodyl CompoundSingle crystals of (IO2)2S2O7 were obtained for the first time by reacting iodic acid and oleum at 195°C. According to the results of a X-ray structure determination (monoclinic, P21/a, a = 885.0(2), b = 1037.3(2), c = 915.8(2) pm, β = 94.75(2)°, Z = 4, 1466 diffractometer data, R1 = 0.033, wR2 = 0.063), (IO2)2S2O7 contains dimeric iodyl cations (IO2)22+, which are connected by disulfate groups thus forming polymeric strands. Strikingly, the I—O-distances range almost continously from 174 pm (strong intramolecular bonds) to — 300 pm (van der Waals contacts).
    Notes: Durch Umsetzung von Iodsäure in Oleum bei 195°C wurden erstmals Einkristalle von Iodyldisulfat erhalten. Nach der Röntgenstrukturanalyse (monoklin, P21/a, a = 885,0(2), b = 1037,3(2), c = 915,8(2) pm, β = 94,75(2)°, Z = 4, 1466 unabhängige Reflexe, R1 = 0,033, wR2 = 0,063) liegen dimere Iodylkationen (IO2)22+ vor, die über Disulfatgruppen zu polymeren Strängen verknüpft sind. Auffällig ist eine nahezu gleichmäßige Verteilung der I—O-Abstände über den gesamten Bereich von starken intramolekularen Bindungen (174 pm) bis zu intermolekularen Kontakten vom van der Waals Typ (〉 300 pm).
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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