Dimethyltrithiocarbonate reacts with the superacidic systems HF/MF(5) and DF/MF(5) (M = As, Sb) to form (MeS)(2)CSX(+)MF(6)(-) (X = H, D). With an excess of AsF(5) the reaction leads to (MeS)(2)CSX(+)As(2)F(11)(-) (X = H, D). The latter salt crystallizes in the monoclinic space group P2(1)/c (No. 14 with a = 7.687(1) Å, b = 21.327(6) Å, c = 8.704(1) Å, and beta = 91.99(1) degrees ) with four formula units per cell. The undecafluorodiarsenate anion contains an As-F-As bridge with two As-F bonds significantly longer than the nonbridging bonds and an As-F-As angle of 159.1(6) degrees. The Raman, IR, and (1)H, (75)As, (19)F, and (13)C NMR spectra of (MeS)(2)CSX(+)SbF(6)(-) and (MeS)(2)CSX(+)As(2)F(11)(-) (X = H, D) are reported.
Die Darstellung einer Reihe von Dichlor ammoniumsalzen des Typs CH3S(O)2NCl2X+MF6− (X = CH3, Cl, F; M = As, Sb) wird angegeben. Die Salze werden durch oxidative Halogenierung bzw. Methylierung von CH3S(O)2NCl2 erhalten. Die Charakterisierung der thermolabilen Verbindungen erfolgte mittels IR‐, Raman‐sowie Multikern‐NMR‐Spektroskopie. Die Einkristallröntgenstrukturanalyse von N,N‐Dichlormethylsulfonamid CH3S(O)2NCl2 bei 173(1) K ergab: orthorhombische Raum gruppe Pnma mit a = 615,1(3) pm, b = 937,3(5) pm, c = 970,3(5) pm und Z = 4.
Dithiocarbonic acid O,S‐dimethyl ester reacts with the super acidic system HF/MF5 (M = As, Sb) to form (MeO)(MeS)CSX+MF6− (M = As, Sb; X = H, D). (MeO)(MeS)CSH+SbF6− crystallizes in the monoclinic space group P21/n (No. 14) with a = 8.634(2) Å, b = 9.521(3)Å, c = 12.509(4) Å, β = 97.39 (2)° and 4 formula units per cell. The reaction of O,S‐dimethyl dithiocarbonate with the super acidic systems XF/MF5 (X = H, D; M = As, Sb) is discussed with regard to the formation of the salts, and Raman, IR, 1H NMR, and 13C NMR spectra of (MeO)(MeS)CSX+MF6− (M = As, Sb; X = H, D) are reported.
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