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  • 1
    ISSN: 0044-2313
    Keywords: Ruthenium ; boranes ; organoruthenaboranes ; preparation ; mass, n.m.r. spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Organoruthenaboran-Chemie. IX. Die Reaktion von [{(η6-C6Me6)RuCl2}2] und [{(η6-MeC6H4-4-iPr)RuCl2}2] mit dem [nido-B9H12]--AnionDie Reaktion zwischen [NnBu4][nido-B9H12] und [{(η6-C6Me6)RuCl2}2] in CH2Cl2-Lösung ergibt [5-Cl-6-(η6-C6Me6)-nido-6-RuB9H12] (12%), [6-(η6-C6Me6)-nido-6-RuB9H13] (1%) und [1-(η6-C6Me6)-isocloso-1-RuB9H9] (2%). Die entsprechende Reaktion mit dem p-Cymol-Analogon [{(η6-MeC6H4-iPr)RuCl2}2] ergibt [5-Cl-6-(η6-MeC6H4-4-iPr)-nido-6-RuB9H12] (15%), [6-(η6-MeC6H4-4-iPr)-nido-6-RuB9H13] (1%) und [1-(η6-MeC6H4-4-iPr)-isocloso-1-RuB9H9] (3%). Die Produkte sind gelbe, luftstabile Festkörper; sie wurden chromatographisch getrennt und massenspektroskopisch und NMR-spektroskopisch charakterisiert.
    Notes: Reaction between [NnBu4][nido-B9H12] and [{(η6-C6Me6)RuCl2}2] in CH2Cl2 solution yields [5-Cl-6-(η6-C6Me6)-nido-6-RuB9H12] (12%), [6-(η6-C6Me6)-nido-6-RuB9H13] (1%), and [1-(η6-C6Me6)-isocloso-1-RuB9H9] (2%). The corresponding reaction with the p-cymene analogue [{(η6-MeC6H4-4-iPr)RuCl2}2] yields [5-Cl-6-(η6-MeC6H4-4-iPr)-nido-6-RuB9H12] (15%), [6-(η6-MeC6H4-4-iPr)-nido-6-RuB9H13] (1%), and [1-(η6-MeC6H4-4-iPr)-isocloso-1-RuB9H9] (3%). The products were all yellow, air-stable solids; they were separated by chromatography and characterized by mass spectrometry and n.m.r. spectroscopy.
    Additional Material: 2 Ill.
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  • 2
    ISSN: 0044-2313
    Keywords: Organoruthenaboranes ; ruthenium ; boranes ; n.m.r. spectra ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Organoruthenaboran-Chemie. X. Die SMe2-katalysierte Bildung von [1-(η6-C6Me6)-isocloso-RuB9H9] und einige B-Phenylamino-Derivate. NMR- und Röntgen-UntersuchungenDie Einwirkung von SMe2, auf das zehneckige nido-Ruthenaboran [1-(η6-C6Me6)RuB9H13] (1) führt in hoher Ausbeute zum unsubstituierten isocloso-Ruthenaboran [1-(η6-C6Me6)RuB9H9] (2). Die analoge Verbindung mit Benzol [1-(η6-C6Me6)RuB9H9] wird entsprechend erhalten. Im Gegensatz dazu führt die Reaktion von (1) mit PhNH2 zu einer Reihe von B-Phenylamino-isocloso-Derivaten wie [1-(η6-C6Me6)-2-(PhNH)-isocloso-1-RuB9H8] (3) (orange Kristalle), [1-(η6-C6Me6)-2,3-(PhNH)2-isocloso-1-RuB9H7] (4) (rotorange) und [1-(η6-C6Me6)-5,6,7-(PhNH)3-isocloso-l-RuB9H6] (5) (dunkelrot). Detaillierte 1H- und 11B-NMR-Spektren werden angegeben. Die Struktur von (3) wird durch eine Einkristall-Röntgen-Strukturanalyse des Solvats [1-(η6-C6Me6)-2-(PhNH)-isocloso-1-RuB9H8] · 1/2 CH2C12 ermittelt; die Kristalle sind monoklin, Raumgruppe C2/c, mit a = 1895,1(3), b = 1556,6(3), c = 1716,4(3)pm, β = 104,37(1)° und Z = 8.
    Notes: The action of SMe2 on the ten-vertex nido-ruthenaborane [6-(η6-C6Me6)RuB9Hl3] (1) provides a high-yield route to the unsubstituted isocloso-ruthenaborane [1-(η6-C6Me6)RuB9H9] (2). The benzene analogue [1-(η6-C6Me6)RuB9H9] is prepared similarly. By contrast, reaction of (1) with PhNH2 gives a variety of B-phenylamino isocloso derivatives, including orange crystals of [1-(η6-C6Me6)-2-(PhNH)-isocloso-1-RuB9H8] (3), red-orange [1-(η6-C6Me6)-2,3-(PhNH)2-isocloso-1-RuB9H7] (4) and dark-red [1-(η6-C6Me6)-5,6,7-(PhNH)3-isocloso-1-RuB9H6] (5). Detailed 1H and 11B nmr properties of these various compounds are described. The structure of (3) has been established by a single-crystal X-ray diffraction study of the solvate [1-(η6-C6Me6)-2-(PhNH)-isocloso-1-RuB9H8] · 1/2 CH2Cl2; the crystals were monoclinic, space group C2/c, with a = 1895.1(3), b = 1556.6(3), c = 1716.4(3) pm, β = 104.37(1)° and z = 8.
    Additional Material: 2 Ill.
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  • 3
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Polyedrische Ruthenaboran-Chemie: Darstellung, Molekularstruktur und NMR-Eigenschaften der ligandengemischten, elfeckigen isocloso-Verbindung [1,1-(PMe3) (PPh3)-closo-1-RuB10H8-2,3-(OEt)2]Umsetzung von [1,1-(PPh3)2-closo-1-RuB10H8 -2,3-(OEt)2]1) 1 mit dem basischeren Liganden PMe3 ersetzt leicht das PPh3 unter Bildung der bisher nicht mitgeteilten ligandengemischten Verbindung [1,1-(PMe3) (PPh3)-closo-1-RuB10H8-2,3-(OEt)2] 2, die durch Einkristall Röntgen-Analyse charakterisiert wird. Die Kristalle sind monoklin, Raumgruppe P21, mit a = 1059,2(2), b = 1291,5(2), c = 1187,6(2) pm, β = 91,56(1)°, Z = 4; dem endlich R = Faktor von 0,0198 für 3303 beobachtete Reflexe [I〉2,0 s̰(I)]. Verbindung 2 wird ferner charakterisiert durch detaillierte Mehrkern-, Mehrfachresonanz- und Mehrdimensionale-NMR-Spektroskopie (1H, 1H-{11B}, [1H-1H] {11B}-COSY, 11B-{1H} und 31P).
    Notes: Treatment of [1,1-(PPh3)2-closo-1-RuB10H8-2, 3-(OEt)2]1) 1 with the more basic ligand PMe3 readily results in the displacement of PPh3 to form the hitherto unreported mixed ligand compound [1,1-(PMe3) (PPh3)-closo-1-RuB10H8-2, 3-(OEt)2] 2, which is characterized by singlecrystal X-ray diffraction analysis. Crystals are monoclinic, space group P21, with a = 1059.2(2), b = 1291.5(2), c = 1187.6(2) pm, β = 91.56(1)°, Z = 4; the final R factor is 0.0198 for 3303 observed reflections [I〉2.0 s̰(I)]. Compound 2 is also characterized by detailed multielement, multiple resonance, and multidimensional n.m.r. spectroscopy (1H, 1H-{11B}, [1H-1H]{11B}-COSY, 11B, 11B-{1H}, and 31P).
    Additional Material: 4 Ill.
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  • 4
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Organoruthenaboran Chemie. VIII. Die Reaktionen von [{(η6-C6Me6)RuCl2}2] und [{(η6-MeC6H4Pr)RuCl2}2] mit Cs[arachno-6-SB9H12]: Isolierung von zehn-, elf- und zwölfeckigen Ruthenathiaboranen und ihre Charakterisierung durch NMR-SpektroskopieDie Reaktion von [{(η6-C6H6)RuCl2}2] mit arachno-[6-SB9H12]- und NaH in CH2Cl2/Aceton-Lösung ergibt in niedriger Ausbeute (1,3%) ein closo-zehneckiges Ruthenathiaboran, [2-(η6-C6Me6)-closo-2, 1-RuSB8H8], während die Reaktion des p-Cymolanalogon [{(η6-MeC6H4Pr)RuCl2}2] mit arachno-[6-SB9H12]- und N,N,N′,N′ Tetramethylnaphthalin-1,8-diamin(tmnd) in Aceton nido-elfeckige und closo-zwölfeckige Ruthenathiaborane folgender Formulierungen [11-Cl-7-(η6MeC6H4Pr)-nido-7, 8-RuSB9H10] (2,2%), [2,3-(η6-MeC6H4Pr)2 -closo-2,3,1-Ru2SB9H9] (21%), und [7-Cl-2, 3-(η6MeC6H4Pr)2-closo -2,3,1-Ru2SB9H8] (8%) ergibt. Die Produkte sind alle luftstabile, rote oder gelbe Festkörper und werden durch kernmagnetische Doppelresonanz und 2D-Korrelations-NMR-Spektroskopie (COSY) charakterisiert.
    Notes: Reaction of [{(η6-C6H6)RuCl2}2] with arachno-[6-SB9H12]- and NaH in CH2Cl2/acetone solution gives a low yield (1.3%) of a closo ten-vertex ruthenathiaborane formulated as [2-(η6-C6Me6)-closo-2,1-RuSB8 H8] whereas reaction of the p-cymene analogue [{(η6-MeC6H4Pr)RuCl2}2] with arachno-[6-SB9H12]- and N,N,N′,N′-tetramethylnaphalene-1,8-diamine (tmnd) in acetone yields nido-eleven-vertex and closo-twelve-vertex ruthenathiaboranes of proposed formulations [11-Cl-7-(η6MeC6H4Pr)-nido-7, 8-RuSB9H10] (2.2%), [2,3-(η6-MeC6H4Pr)2- closo-2,3,1-Ru2SB9H9] (21%), and [7-Cl-2,3-(η6-MeC6H4Pr)2 -closo-2,3,1-Ru2SB9H8] (8%). The products are all air-stable red or yellow solids and their characterization made use of nuclear magnetic double resonance and twodimensional correlation n.m.r. spectroscopy (COSY).
    Additional Material: 6 Ill.
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  • 5
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für die chemische Industrie 83 (1971), S. 746-755 
    ISSN: 0044-8249
    Keywords: Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Nach einem Überblick über die Einflüsse auf die Isomerieverschiebung von Gammaresonanzlinien, ihre elektrische Quadrupolaufspaltung sowie auf die magnetische Dipolaufspaltung werden Anwendungsbeispiele der Gammastrahlen-Resonanzspektroskopie (Mößbauer-Spektroskopie) für Festkörpersysteme beschrieben. Anhand neuer Ergebnisse für die ungeordneten Rutil-Phasen Fe2MgF6, FeMg2F6 und FeCoNiF6 und für die Trirutil-Phase LiFeIIFeIIIF6 lassen sich die Vorteile dieser Methode zur Untersuchung von Festkörpern hinsichtlich des Oxidationszustandes, der Punktsymmetrie und der magnetischen Ordnung aufzeigen. Resultate einer eingehenden Untersuchung der nicht-stöchiometrischen Wüstit-Phase Fe1—xO werden durch diffusionsbedingte Linienverbreiterung bei hoher Temperatur und durch Bildung von Fehlstellen-Cluster in den abgeschreckten Proben erklärt; die Entstehung von im wesentlichen stöchiometrisch zusammengesetztem FeO durch Ausheilung wird diskutiert. Zur Anwendung starker äußerer Magnetfelder auf diamagnetische Zinnverbindungen werden aktuelle Befunde mitgeteilt, ebenso wie die einer Mößbauer-Untersuchung an Mondproben, welche von Apollo 11 und 12 zur Erde gebracht wurden.
    Additional Material: 13 Ill.
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  • 6
    ISSN: 0749-1581
    Keywords: closo-Metalladicarbaborane ; 11B assignments ; Proton-boron shift correlation ; Ruthenium ; Cluster ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The cluster 11B chemical shifts in members of the important class of closo-3,1,2-metalladicarbaboranes were previously unassigned, and their cluster 1H chemical shifts previously unmeasured. The use of [11B—11B]-COSY and 1H-{11B} NMR spectroscopy to measure and assign the cluster 11B and 1H chemical shifts of (previously unreported) [3-(η6-C6Me6)-closo-3,1,2-RuC2B9H11] as a model compound is reported. The 11B shielding patterns of this species and the nonmetalla simple carbaborane analogue [1,2-C2B10H12] are compared and briefly discussed.
    Additional Material: 2 Ill.
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  • 7
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Angewandte Chemie International Edition in English 10 (1971), S. 716-724 
    ISSN: 0570-0833
    Keywords: Moessbauer spectroscopy ; Solid-state reactions ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The factors influencing the chemical isomer shift, quadrupole splitting and hyperfine magnetic interactions, are briefly summarized and applications to solid state systems reviewed. New results on the disordered rutile phases Fe2MgF6, FeMg2F6, and FeCoNiF2, and on the trirutile phase Li+ Fe2+ Fe3+ F6 are presented to illustrate the power of the Mössbauer technique in probing details of oxidation states, site symmetries and magnetic ordering. An extensive study on the nonstoichiometric wüstite phase Fe1-xO is also reported and analyzed in terms of diffusion broadening at high temperatures and defect clustering in quenched samples; the production of essentially stoichiometric FeO by annealing is also discussed. Recent results on the application of large external magnetic fields to diamagnetic compounds of tin are reviewed and results of a Mössbauer investigation of lunar samples returned by the Apollo 11 and 12 missions are discussed.
    Additional Material: 13 Ill.
    Type of Medium: Electronic Resource
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