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  • 1
    ISSN: 0044-2313
    Keywords: Ethylenedithiobis(dimethylsulfonium) Salts ; Bisdimethylsulfoniumtrithiocarbon Acid Diester Bishexachloroantimonate ; IR Spectra ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Reaction of Chloromethylsulfonium Salts with Ethanedithiol and Trithiocarbon Acid and Crystal Structure of 2-Methyl-1,2,3-trithiolaniumhexachloroantimonateBy simple condensation reactions among chlorodimethylsulfonium salts and ethanedithiol or trithiocarbon acid the ethylenedithiobis(dimethylsulfonium) salts [(CH3)2S—S—(CH2)2—S—S(CH3)2]2+ (SbCl6-)2 and (HSO4-)2 respectively the bisdimethylsulfoniumtrithiocarbonaciddiester-bishexachloroantimonate [(CH3)2S—S—C(S)—S—S(CH3)2]2+ (SbCl6-)2 are obtained.From dichloromethylsulfoniumhexachloroantimonate and ethanedithiol the S-methylated 1,2,3-trithiolaniumhexachloroantimonate is formed. Its crystal structure is reported. It crystal structure is reported. It crystallizes in the space group P1 with a = 672.2 pm, b = 782.3 pm, c = 1335.3 pm, α = 87.40°, β = 83.07d, g = 89,18°, V = 696×06 pm3 and Z = 2. The five-ring is wave-like with an upset SSS angle and a ring-spaned S2-S3 contact.
    Notes: Durch einfache Kondensationsreaktionen zwischen Chlordimethylsulfoniumsalzen und Ethandithiol bzw. Trithiokohlensäure werden die Ethylendithiobis(dimethylsulfonium)salze [(CH3)2S—S—(CH2)2—S—S(CH3)2]2+ (SbCl6-)2 und (HSO4-)2 bzw. das Bisdimethyl-sulfoniumtrithiokohlensäurediesterbishexachloroantimonat [(CH3)2S—S—C(S)—S—S(CH3)2]2+ (SbCl6-)2 erhalten.Aus Dichlormethylsulfoniumhexachloroantimonat und Ethandithiol entsteht das S-methylierte 1,2,3-Trithiolaniumhexachloroantimonat, dessen Kristallstruktur mitgeteilt wird. Es kristallisiert in der Raumgruppe P1 mit a = 672,2 pm, b = 782,3 pm, c = 1335,3 pm, α = 87,40°, β = 83,07°, γ = 89,18°, V = 696 · 106 pm3, Z = 2. Der Fünfring ist gewellt mit einem gestauchten SSS-Winkel und einem ringüberbrückenden S2-S3-Kontakt.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 0044-2313
    Keywords: Chromium ; Palladium ; Copper Phosphaneimine Complexes ; Syntheses ; IR Spectra ; Crystal Structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Silylated Phosphaneimine Complexes of Chromium(II), Palladium(II), and Copper(II). The Crystal Structures of [CrCl2(Me3SiNPMe3)2], [PdCl2(Me3SiNPEt3)2], and [CuCl2(Me3SiNPMe3)]2The title compounds have been prepared by the reaction of the silylated phosphaneimines Me3SiNPR3 (R = CH3, C2H5) with CrCl2(THF)2, PdCl2 and CuCl2, respectively, in dichloromethane suspensions. All donor-acceptor complexes were characterized by IR spectroscopy and by crystal structure determinations.[CrCl2(Me3SiNPMe3)2]: Space group Pccn, Z = 4, structure determination with 2104 observed unique reflections, R = 0.045. Lattice dimensions at -70°C: a = 1326.3, b = 1562.5, c = 1171.5 pm. Within the monomeric molecular structure the chromium atom is planarly coordinated within the trans-configuration of the Cl atoms and the N atoms with distances of Cr—Cl = 235.94 pm and Cr—N = 211.7 pm.[PdCl2(Me3SiNPEt3)2]: Space group P21/n, Z = 2, structure determination with 2412 observed unique reflections, R = 0.031. Lattice dimensions at 20°C: a = 917.3, b = 1390.2, c = 1161.7 pm, β = 95.80°. Within the monomeric molecular structure the palladium atom is planarly coordinated within the trans-configuration of the Cl atoms and the N atoms with distances of Pd—Cl = 222.9 pm and Pd—N = 209.5 pm.[CuCl2(Me3SiNPMe3)2]: Space group Pbca, Z = 4, structure determination with 1861 observed unique reflections, R = 0.067. Lattice dimensions at -70°C: a = 1440.2, b = 1205.1, c = 1536.5 pm. The compound forms centrosymmetric dimeric molecules, in which the Cu atoms are linked via almost symmetrical chloro-bridges with Cu—Cl distances of 231.4 pm. The distance Cu—N is 196.7 pm.
    Notes: Die Titelverbindungen entstehen bei der Einwirkung der silylierten Phosphanimine Me3SiNPR3 (R = CH3, C2H5) auf CrCl2(THF)2, PdCl2 und CuCl2 in Dichlormethan-Suspension. Die drei Donor-Acceptor-Komplexe werden durch ihre IR-Spektren und durch Kristallstrukturanalysen charakterisiert.[CrCl2(Me3SiNPMe3)2]: Raumgruppe Pccn, Z = 4, Strukturlösung mit 2104 unabhängigen beobachteten Reflexen, R = 0,045. Gitterkonstanten bei -70°C: a = 1326,3; b = 1562,5; c = 1171,5 pm. In der monomeren Molekülstruktur ist das Chromatom planar in der trans-Konfiguration von den Cl-Atomen und den N-Atomen der Phosphanimin-Liganden koordiniert mit Abständen Cr—Cl = 235,94 pm und Cr—N = 211,7 pm.[PdCl2(Me3SiNPEt3)2]: Raumgruppe P21/n, Z = 2, Strukturlösung mit 2412 unabhängigen beobachteten Reflexen, R = 0,031. Gitterkonstanten bei 20°C: a = 917,3; b = 1390,2; c = 1161,7 pm, β = 95,80°. In der monomeren Molekülstruktur ist das Palladiumatom planar in der trans-Konfiguration von den Cl-Atomen und den N-Atomen der Phosphaniminliganden koordiniert mit Abständen Pd—Cl = 222,9 pm und Pd—N = 209,5 pm.[CuCl2(Me3SiNPMe3)]2: Raumgruppe Pbca, Z = 4, Strukturlösung mit 1861 unabhängigen beobachteten Reflexen, R = 0,067. Gitterkonstanten bei -70°C: a = 1440,2; b = 1205,1; c = 1536,5 pm. Die Verbindung bildet zentrosymmetrische dimere Moleküle, in denen die Cu-Atome über nahezu symmetrische Chlorobrücken mit Cu—Cl-Abständen von 231,4 pm verknüpft sind. Der Abstand Cu—N beträgt 196,7 pm.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
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