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  • 1995-1999  (6)
  • 1997  (6)
  • 1
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1633-1638 
    ISSN: 0044-2313
    Keywords: (CH3)2S derivatives ; Structure ; Spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: (CH3)2SBr2 - Reactions and Structures(CH3)2SBr2 (1) is a donor acceptor complex (8-S-3 + 10-Br-2) which reacts with (CH3)2S(=O)NSi(CH3)3 to yield [(CH3)2S(O)=N—S(CH3)2]+Br- (2). With SbBr3 (CH3)2SBr+SbBr4- (3) can be isolated. 1 crystallizes monoclinic in the space group P21/c with a = 733.8, b = 734.2, c = 1132.7 pm, β = 92.8° and Z = 4. 2 crystallizes in the orthorhombic space group Pnma with a = 967.2, b = 793.3, c = 1168.3 pm and Z = 4. The SBr and BrBr force constants of 1 are compared with those of S2Br2, 3 and Br2 resp. The nmr and mass spectra of 1 and 2 are communicated.
    Notes: (CH3)2SBr2 (1) ist ein (8-S-3 + 10-Br-2) Donor-Akzeptor-Komplex(8-S-3 + 10-Br-2) bedeutet: acht Valenzelektronen am S-Atom, das von drei Bindungspartnern umgeben ist, und zehn Valenzelektronen am Br-Atom, das zwei Bindungspartner hat; s.: S. W. Perkins, J. C. Martin, A. J. Arduengeo III, W. Lau, A. Alegria, J. K. Kochi, J. Am. Chem. Soc. 1980, 102, 7753. und reagiert mit (CH3)2S(=O)NSi(CH3)3 zu [(CH3)2S(O)=N—S(CH3)2]+Br- (2), mit SbBr3 zu (CH3)2SBr+SbBr4- (3). 1 kristallisiert monoklin (P21/c) mit a = 733,8, b = 734,2, c = 1132,7 pm, β = 92,8° und Z = 4. 2 kristallisiert orthorhombisch in der Raumgruppe Pnma mit a = 967,2, b = 793,3, c = 1168,3 pm und Z = 4. Die SBr- und BrBr-Kraftkonstanten von 1 werden mit denen von S2Br2 und 3 bzw. Br2 verglichen. Die NMR- und Massenspektren von 1 und 2 werden kurz diskutiert.
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  • 2
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1455-1466 
    ISSN: 0044-2313
    Keywords: Tris(trimethylsilyl)methyl-derivatives, Lithium, Aluminium, Gallium, Indium ; spectra ; X-ray Structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Base-free Tris(trimethylsilyl)methyl Derivatives of Lithium, Aluminium, Gallium, and IndiumBase-free LiR* (R*=-C(SiMe3)3) has been prepared from R*Cl and Li-metal in toluene at 85-90°C and used to synthesize the metallanes R*MMe2 with M = Al, Ga and In, respectively. The NMR (1H, 13C, 29Si) and the vibrational spectra of these trisyl compounds have been discussed.AlCl3 and LiR*(ratio 1 : 1) forms the metallate metallate Li[R*AlCl3]. The triclinic unit cell (space group P1) consists of a centrosymmetric assoziate, formed by four Li[R*AlCl3]- units with Al—Cl…Li bridges, two pairs of Li-atoms differing in their chlorine-coordination and two disordered toluene molecules, inserted in the crystal lattice (R1wR2 =0,0444/0,1072).The reaction of GaCl3 with LiR* (I :1) gives the unusual sesquichloride (R*Ga(Cl1,33)Me0,67)3 in moderate yield. The X-ray structure determination shows a Ga3Cl3-skeleton with chairconformation and disordered, terminal gallium ligands (R1/wR2= 0,0646/0,2270).
    Notes: Basefreies LiR* (R*=-C(SiMe3)3) wurde aus R*Cl und Lithiummetall in Toluol bei 85-90°C erhalten und zur Darstellung der Dimethylmetallane R*MMe2 mit M = Al, Ga, In verwendet, die durch NMR- (1H, 13C, 29Si) und Schwingungsspektren (Raman, IR) charakterisiert werden.AlCl3 und LiR* (Molverhältnis 1 : 1) bilden das Metallat Li[R*AlCl3]. Die trikline Einheitszelle (Raumgruppe P1) enthält ein zentrosymmetrisches, über Al—Cl … Li—Brücken gebildetes Assoziat aus vier Li[R*AlCl3]-Einheiten, mit zwei paarweise unterschiedlich von Chlor koordinierten Li-Atomen sowie zwei fehlgeordnete Toluolmoleküle (R1/ wR2 = 0,0444/0,1072).Die Reaktion von GaCl3 mit LiR* (1 : 1) in Toluol führt in mäßiger Ausbeute zum ungewöhnlichen Sesquichlorid (R*Ga(Cl1,33)Me0,67)3. Die Röntgenstrukturanalyse zeigt ein sesselförmig gewelltes Ga3Cl3-Sechsringgerüst und fehlgeordnete, terminale Liganden am Galliumatom (R1/ wR2 = 0,0646/0,2270).Li[R*AlCl3]. The triclinic unit cell (space group P1) consists of a centrosymmetric assoziate, formed by four Li[R*AlCl3]-units with Al-Cl … Li bridges, two pairs of Li-atoms differing in their chlorine-coordination and two disordered toluene molecules, inserted in the crystal lattice (R1/wR2 = 0,0444/0,1072).The reaction of GaCl3 with LiR* (1 : 1) gives the unusual sesquichloride (R*Ga(Cl1,33)Me0,67)3 in moderate yield. The X-ray structure determination shows a Ga3Cl3-skeleton with chairconformation and disordered, terminal gallium ligands (R1/wR2 = 0,0646/0,2270).
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1168-1174 
    ISSN: 0044-2313
    Keywords: Sulfoximide ; Sulfoximidium Salts ; Structure ; Hydrogenbonding ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Sulfoximide and Sulfoximidium Salts - Structures and Hydrogen BondingIn the solid state dimethylsulfoximide (1) (orthorhombic; space group Pbca; a = 577.8, b = 931.2 and c = 1645.6 pm) makes intermolecular N—H ≡ N hydrogen bonds. The hydrogen halide salts (CH3)2S(O)NH2+Hal- ((2), Hal-=Cl-; (4), Hal-=Br-) reacts with metal halides to yield (CH3)2S(O)NH2+MHalyn- with the complex anions ((5), MHalyn-=SbCl4-; (6), MHalyn-=SbCl52-; (7), MHalyn-=SbCl6-; (8), MHalyn-=SbBr52-; (9), MHalyn-=AlCl4-). 2 crystallizes from ethanol (96%) as [(CH3)2S(O)NH2+Cl-]2 · H2O (3). The structures of 3 (monoclinic; space group P21/c; a = 917.0, b = 1344.7, c = 1080.8 pm and β = 103.8°; Z = 10), 4 (orthorhombic; space group Pbcn; a = 1028.9, b = 1132.6, c = 1074.1 pm; Z = 8) and 6 (monoclinic; space group C2/c; a = 2041.1, b = 1101.4, c = 3365.6 pm and β = 153.8°; Z = 8) are determined by X-ray analysis. In 6 Sb is coordinated in a distorted octahedra by 6 Cl in three short (mean 245,5 pm; SbCl3) and three long distances (291 to 299 pm; Cl-). Two of the chloride ions connect the Sb atoms to infinite Sb … Cl … Sb chains. Except for 7 and 9 there are bridges between the NH2 groups and the halide ions. The NH valence vibrations are discussed in view of hydrogen bonding.
    Notes: Im festen Dimethylsulfoximid (1) (orthorhombisch; Raumgruppe Pbca; a = 577,8, b = 931,2 und c = 1645,6 pm) sind zwischen den Imidgruppen N—H … N-Brückenbindungen ausgebildet. Die mit HHal darstellbaren Salze (CH3)2S(O)NH2+Hal- ((2), Hal-=Cl-; (4), Hal-=Br-) reagieren mit MHalx zu (CH3)2S(O)NH2+MHalyn- ((5), MHalyn-=SbCl4-; (6), MHalyn-=SbCl52-; (7), MHalyn-=SbCl6-; (8), MHalyn-=SbBr52-; (9), MHalyn-=AlCl4-). 2 kristallisiert aus 96% Ethanol als [(CH3)2S(O)NH2+Cl-]2 · H2O (3). Die Strukturen von 3 (monoklin; Raumgruppe P21/c; a = 917,0, b = 1344,7, c = 1080,8 pm und β = 103,8°; Z = 10), 4 (orthorhombisch; Raumgruppe Pbcn; a = 1028,9, b = 1132,6, c = 1074,1 pm; Z = 8) und 6 (monoklin; Raumgruppe C2/c; a = 2041,1, b = 1101,4, c = 3365.6 pm und β = 153,8°; Z = 8) wurden bestimmt. In 6 ist Sb verzerrt oktaedrisch von 6 Cl in drei kurzen (im Mittel 245,5 pm; SbCl3) und drei langen Abständen (291 bis 299 pm; Cl-) umgeben. Zwei der lang gebundenen Cl-Ionen verknüpfen die Sb-Atome zu unendlichen Sb … Cl … Sb-Ketten. Die NH2-Gruppen der Kationen bilden außer in 7 und in 9 H—Brückenbindungen zu den Halogenidionen. Die NH-Valenzschwingungen werden im Hinblick auf die Wasserstoffbrückenbindungen diskutiert.
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  • 4
    Publication Date: 1997-09-01
    Print ISSN: 0044-2313
    Electronic ISSN: 1521-3749
    Topics: Chemistry and Pharmacology
    Published by Wiley
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  • 5
    Publication Date: 1997-10-01
    Print ISSN: 0044-2313
    Electronic ISSN: 1521-3749
    Topics: Chemistry and Pharmacology
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  • 6
    Publication Date: 1997-07-01
    Print ISSN: 0044-2313
    Electronic ISSN: 1521-3749
    Topics: Chemistry and Pharmacology
    Published by Wiley
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