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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.
    Type of Medium: Electronic Resource
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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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