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  • 1
    ISSN: 0044-2313
    Keywords: Cyclic thiophosphate ; cyclic thiochlorosilicate ; dichlorodithiophosphate ; dibromodithiophosphate ; crystal structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Two New Cyclic Thioanions: (PPh4)2[1,3-P2S8] and (PPh4)2[Si2S6Cl2]. New Synthetic Access Routes to PPh4[PS2Cl2] and PPh4[ PS2Br2](PPh4)2[P2S8] was obtained from tetraphenylphosphonium polysulfide and white phosphorus in acetonitrile. According to its X-ray crystal structure analysis (4229 reflexions, R = 0.079) the P2S82- ion consists of a six-membered ring in chair conformation made up from four sulfur and two phosphorus atoms in 1,3 positions; in addition, each P atom has two terminal sulfur atoms. (PPh4)2[Si2S6Cl2] · 2 CH2Cl2 was obtained from Na2S4, PPh4Cl and SiCl4 in dichloromethane. The Si2S6Cl22- ion also has a six-membered ring structure, consisting of four sulfur and two silicon atoms in 1,4 positions (X-ray structure analysis, 2694 reflexions, R = 0.032). PPh4[PS2Cl2] is accessible by the following reactions: 1P4S3 + PPh4Cl + chlorine in CH2Cl2;2PSCl3 + Na2S4 + PPh4Cl in CH2Cl2;3PCl5 + Na2S4 + PPh4Cl in acetonitrile;4PCl3 + Na2S4 + PPh4Cl in acetonitrile;5P4S10 + Na2S4 + PPh4Cl in acetonitrile .P4S3 or react with PPh4Cl and bromine to yield PPh4[PS2Br2]. PPh4[PS2Cl2] crystallizes isotypic to PPh4[PS2Br2] in the BiPh4[ClO4] structure type with orientational disorder of the PS2Cl2- ions in positions with site symmetry 4.
    Notes: Aus Tetraphenylphosphonium-polysulfid und weißem Phosphor wurde in Acetonitril (PPh4)2[1,3-P2S8] hergestellt. Nach seiner Kristallstrukturanalyse mittels Röntgenbeugung (R = 7,9% für 4229 Reflexe) besteht das 1,3-P2S82--Ion aus einem sechsgliedrigen Ringgerüst in Sesselkonformation mit vier Schwefel- und zwei Phosphoratomen in 1,3-Stellung sowie zwei terminalen Schwefelatomen an den P-Atomen. (PPh4)2[Si2S6Cl2] · 2 CH2CI2 wurde aus Na2S4, PPh4Cl und SiCl4 in Dichlormethan erhalten. Das Si2S6Cl22--Ion hat ebenfalls ein sechsgliedriges Ringgerüst in Sesselkonformation, bestehend aus vier Schwefel- und zwei Si-Atomen in 1,4-Stellung (Röntgenstrukturanalyse mit 2694 Reflexen, R = 3,2%). Mit folgenden fünf Syntheseverfahren läßt sich PPh4[PS2Cl2] herstellen: 1P4S3 + PPh4Cl + Chlor in CH2Cl2;2PSCl3 + Na2S4 + PPh4Cl in CH2Cl2;3PCl5 + Na2S4 + PPh4Cl in Acetonitril4PCl3 + Na2S4 + PPh4Cl in Acetonitril5P4S10 + Na2S4 + PPh4Cl in Acetonitril.Aus P4S3 oder P4S10, PPh4Cl und Brom ist PPh4[PS2Br2] zugänglich. PPh4[PS2Cl2] kristallisiert isotyp zu PPh4[PS2Br2] im BiPh4[ClO4]-Typ, mit fehlgeordneten PS2Cl2--Ionen in Punktlagen der Symmetrie 4.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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