ALBERT

All Library Books, journals and Electronic Records Telegrafenberg

feed icon rss

Your email was sent successfully. Check your inbox.

An error occurred while sending the email. Please try again.

Proceed reservation?

Export
  • 1
    ISSN: 0044-2313
    Keywords: Chalcogeno-fluorotungstates ; syntheses ; i.r. spectra ; crystal structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Chalcogeno-Fluoro-Tungstates. The crystal Structures of [Na-15-Crown-5]2[WO2F3]2 ·2 CH3CN and [Na-15-Crown-5]2[WOSF3]2 · 2 CH3CNThe reaction of sodium fluoride with WSCL4 in acetonitrile solution successively leads in the presence of 15-crown-5 to the complexes [Na-15-crown-5][WSCl4F], [Na-15-crown-5]2[WSCl2F3], and [Na-15-crown-5][WSF5]. These complexes are characterized by their i.r. spectra. In acetonitrile partial hydrolysis of [Na-15-crown-5][WSF5] leads to [Na-15-crown-5]2[WSOF3]2 · 2 CH3CN; likewise one obtains [Na-15-crown-5]2[WO2[WO2F3]2] · 2 CH3CN from [Na-15-crown-5]2[WSOF7] by partial hydrolysis. X-ray structural analyses were carried out for both these chalcogeno complexes. [Na-15-crown-5]2[WO2F3]2 · 2 CH3CN: space group P1, Z = 1, 2316 unique observed reflexions, R = 0.036. Lattice dimensions at -65°C: a = 851.0, b = 1064.6, c = 1130.2 pm, α = 105.18°, β = 95.12°, γ = 102.48°.[Na-15-crown-5]2[WOSF3]2 · 2 CH3CN: space group P1, Z = 1,2472 unique observed reflexions, R = 0.030. Lattice dimensions at -80°C: a = 856.3, b = 1062.8, c = 1181.1 pm, α = 107.68°, β = 95.52°, γ = 102.65°.Both compounds are isotypical with each other; they form ion triples which originate from two short Na…F-contacts of 232 pm each with the four axially arranged fluorine ligands of the dimeric anions [WO2F3]22- and [WSOF3]22-, respectively. The dimerization takes place via angular fluoro bridges with W—F-bondings which are only slightly differing in length. The chalcogeno ligands are in the trans-positions to the bridging fluorine atoms.
    Notes: Die Reaktion von Natriumfluorid mit WSCl4 in Acetonitrillösung führt in Gegenwart von 15-Krone-5 schrittweise zu den Komplexen [Na-15-Krone-5][WSCl4F], [Na-15-Krone-5][WSCl2F3] und [Na-15-Krone-5][WSF5], die durch ihre IR-Spektren charakterisiert werden. Partielle Hydrolyse von [Na-15-Krone-5][WSF5] führt in Acetonitril zu [Na-15-Krone-5]2[WSOF3]2 · 2 CH3CN, ebenso erhält man aus [Na-15-Krone-5][WF7] durch partielle Hydrolyse [Na-15-Krone-5]2[WO2F3]2 · 2 CH3CN. Von beiden Chalkogenokomplexen wurden röntgenographische Strukturanalysen ausgeführt.[Na-15-Krone-5]2[WO2F3]2 · 2 CH3CN: Raumgruppe P1, Z = 1, 2316 unabhängige beobachtete Reflexe, R = 3,6%. Gitterkonstanten bei -65°C: a = 851,0; b = 1064,6; c = 1130,2 pm; α = 105,18°; β = 95,12°; γ = 102,48°. [Na-15-Krone-5]2[WOSF3]2 · 2 CH3CN: Raumgruppe P1, Z = 1, 2472 unabhängige beobachtete Reflexe, R = 3,0%. Gitterkonstanten bei -0°C: a = 856,3; b = 1062,8; c = 1181,1 pm; α = 107,68°; β = 95,52°; γ = 102,65°.Beide Verbindungen sind miteinander isotyp; sie bilden Ionentripel, die durch je zwei kurze Na…F-Kontakte von 232 pm mit den vier axial angeordneten Fluorliganden der dimeren Anionen [WO2F3]22- bzw. [WSOF3]22- zustandekommen. Die Dimerisierung erfolgt über gewinkelte Fluorobrücken mit nur wenig verschieden langen W—F-Bindungen. Die Chalkogenoliganden befinden sich in den trans-Positionen zu den Brücken-F-Atomen.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
  • 2
    ISSN: 0044-2313
    Keywords: Amidinato complexes of thallium(III) ; syntheses ; i.r. spectra ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Trimethylsilyl Substituted Amidinato Complexes of Thallium(III). The Crystal Structure of [Ph—C(NHSiMe3)2] [Ph—C(NSiMe3)2TlCl3]The amidinato complexes [Ph—C(NSiMe3)2TlCl3] and [Ph—C(NHSiMe3)2] [Ph—C(NSiMe3)2TlCl3] have been prepared by the reaction of TlCl3 with N,N,N′-tris(trimethylsilyl)benzamidine in THF solution. They were characterized by IR spectroscopy, [Ph—C(NHSiMe3)2] [Ph—C(NSiMe3)2TlCl3] additionally by an X-ray structure determination. Space group P21/c, Z = 4, 4300 observed unique reflexions, R = 0.053. Lattice dimensions at -43°C: a = 1157.2, b = 2346.3, c = 1536.9 pm, β = 105.98°. The structure consists of amidinium cations, and of anions [Ph—C(NSiMe3)2TlCl3]-, in which the thallium atom is fivefold surrounded by three chlorine atoms and by two nitrogen atoms of the amidinato chelate.
    Notes: Die Amidinatokomplexe [Ph—C(NHSiMe3)2TlCl2] und [Ph—C(NHSiMe3)2TlCl2] [Ph—C(NSiMe3)2TlCl3] entstehen bei der Einwirkung von Thallium(III)-chlorid auf N,N,N′-Tris(trimethylsilyl)benzamidin in Tetrahydrofuranlösung. Sie werden durch ihre IR-Spektren, und [Ph—C(NHSiMe3)2] [Ph—C(NSiMe3)2TlCl3] zusätzlich durch eine Kristallstrukturanalyse charakterisiert. Raumgruppe P21/c, Z = 4, 4300 unabhängige beobachtete Reflexe, R = 5,3%. Die Gitterkonstanten betragen bei -43°C: a = 1157,2; b = 2346,3; c = 1536,9 pm; β = 105,98°. Die Verbindung besteht aus einem Amidiniumkation und einem [Ph—C(NSiMe3)2TlCl3]--Anion, in dem das Thalliumatom verzerrt trigonal-bipyramidal von drei Cl-Atomen und chelatartig von den beiden N-Atomen des Amidinatoliganden umgeben ist.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
  • 3
    ISSN: 0044-2313
    Keywords: Crown ether complexes ; tellurium ; antimony ; syntheses ; i.r. spectra ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Crown Ether Complexes [K(15-Crown-5)2]3[Sb3I12], [TeCl3(15-Crown-5)][TeCl5], and [TeCl3(15-Crown-5)]2[TeCl6]Orange-coloured crystals of [K(15-crown-5)2]3[Sb3I12] are formed in the reaction of potassium iodide with antimony triiodide and 15-crown-5 in acetonitrile solution. An X-ray structure determination reveals severe disorder of the crown ether molecules, which coordinate to the potassium atoms in a sandwich array; so only the [Sb3I12]3- ion and the potassium positions were ascertained. The anion is a centrosymmetric trimer (symmetry C2h), which can be understood as central SbI63- ion, coordinated by two SbI3 molecules. (Space group C2/m), Z = 2, 3263 observed, independent reflections, R = 0.06, lattice dimensions at 20°C: a = 2541.1 pm, b = 1441.7 pm, c = 1588.4 pm, β = 113.33°.The tellurium complexes [TeCl3(15-crown-5)] [TeCl5] and [TeCl3(15-crown-5)]2[TeCl6] are prepared by reaction of TeCl4 with 15-crown-5 in acetonitrile solution, forming yellow-green crystals sensitive to moisture. They are characterized by their i.r. spectra.
    Notes: Orange Kristalle [K(15-Krone-5)2]3[Sb3I12] entstehen durch Einwirkung von Kaliumiodid auf Antimontriiodid bei Anwesenheit von 15-Krone-5 in Acetonitrillösung. Wegen Fehlordnung der die Kaliumionen sandwichartig koordinierenden Kronenethermoleküle konnten röntgenogrpahisch in der Struktur nur das [Sb3I12]3--Ion sicher aufgeklärt werden. Es bildet ein zentrosymmetrisches Trimer (Symmetrie C2h), das sich als zentrales SbI63--Ion mit zwei koordinierten SbI3-Molekülen auffassen läßt. Raumgruppe C2/m, Z = 2, 3263 unabhängige beobachtete Reflexe, R = 6,2%. Gitterabmessungen bei 20 °C: a = 2541,1; b = 1441,7; c = 1588,4 pm, β = 113,33°.Die Tellurokomplexe [TeCl3(15-Krone-5)] [TeCl5] und [TeCl3(15-Krone-5)]2[TeCl6] entstehen aus TeCl4 und 15-Krone-5 in Acetonitrillösung als gelbgrüne, feuchtigkeitsempfindliche Kristalle, die durch ihre IR-Spektren charakterisiert werden.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
Close ⊗
This website uses cookies and the analysis tool Matomo. More information can be found here...