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• W1973527290 endingPage "417" @default.
• W1973527290 startingPage "405" @default.
• W1973527290 abstract "O,O′-Diethylthiocarbonat setzt sich mit Bis-(tetrahydrofuran)lithium-bis(trimethylsilyl)phosphanid in 1,2-Dimethoxyethan unterhalb 0°C zu Ethoxy-trimethylsilan und Tris(1,2-dimethoxyethan-O,O′)lithium-2λ3-phosphaethinylsulfanid – [P≡CS]−[Li(dme)3]+ – (1a) Alkylidynephosphanes and -arsanes. I [P ≡ CS]−[Li(dme)3]+ – Synthesis and Structure O,O′-Diethyl thiocarbonate and bis(tetrahydrofuran)-lithium bis(trimethylsilyl)phosphanide dissolved in 1,2-dimethoxyethane, react below 0°C to give ethoxy trimethylsilane and tris(1,2-dimethoxyethane-O,O′)lithium 2λ3-phosphaethynylsulfanide – [P≡CS]− [Li(dme)3]+ – (1a). Apart from bis(trimethylsilyl)sulfane or carbon oxide sulfide, dark red concentrated solutions of λ3-phosphaalkyne 1 are also obtained from reactions of carbon disulfide with bis(tetrahydrofuran)-lithium bis(trimethylsilyl)phosphanide or with the homologous lithoxy-methylidynephosphane (2) [1]. The ir spectrum shows two absorptions at 1762 and 747 cm−1 characteristic for the P≡C and CS stretching vibrations. The nmr parameters {δ(31P) − 121.3; δ(13C) 190.8 ppm; 1JCP 18.2 Hz} resemble much more values of diorganylamino-2λ3-phosphaalkynes than those of bis(1,2-dimethoxyethane-O,O′)lithoxy-methylidyne-phosphane (2a). As found by an X-ray structure analysis (P21/c; a = 1192.6(16); b = 1239.1(19); c = 1414.8(26) pm; β = 105.91(13)° at −100 ± 3°C; Z = 4 formula units; wR = 0.064) of pale yellow crystals (mp. + 16°C) isolated from the reaction with O,O′-diethyl thiocarbonate, the solid is built up of separate [P≡CS]− and [Li(dme)3]+ ions. Typical bond lengths and angles are: P≡C 155.5(11); CS 162.0(11); LiO 206.4(17) to 220.3(20) pm; P≡CS 178.9(7)°." @default.
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• W1973527290 date "1994-03-01" @default.
• W1973527290 modified "2023-09-30" @default.
• W1973527290 title "Alkylidinphosphane und -arsane. I [P ? C?S]?[Li(dme)3]+ - Synthese und Struktur" @default.
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• W1973527290 doi "https://doi.org/10.1002/zaac.19946200303" @default.
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