The preparations of [Mg(NSF3)4](AsF6)2 (2a) and [Zn(NSF3)4](AsF6)2 (2b) are reported. The structure of 2b was determined by X-ray diffraction. The ligand properties of NSF3 are discussed.
The preparations of [Mg(NSF3)(4)](AsF6)(2) (2a) and [Zn(NSF3)(4)](AsF6)(2) (2b) are reported. The structure of 2b was determined by X-ray diffraction. The ligand properties of NSF3 are discussed.
The preparations of [Mg(NSF 3 ) 4 ](AsF 6 ) 2 (2a) and [Zn(NSF 3 ) 4 ](AsF 6 ) 2 (2b) are reported. The structure of 2 b was determined by X-ray diffraction. The ligand properties of NSF 3 are discussed
AbstractBei Umsetzung von "Ihiazylfluorid (I) mit LiN(SiMe3)R′ (R′ : C Me; (II); R′: SiMe3 (VI)) entstehen die linearen und cyclischen Thiazene (III), (IV), (VII), (VIII) bzw. (IX), die isoliert oder nur spektroskopisch nachgewiesen werden.
Nucleophilic substitutions of thiazyl fluoride (NSF) should afford access to thiazyl derivatives RSN. On reaction of NSF with LiOCMe3, the primary product “LiNS(F)OCMe3” could be trapped for the first time as the double cluster 1 and subsequently characterized. A molar ratio of NSF: nucleophile of 1:1 is essential for the formation of 1. equation image
AbstractDie in flüssigem SO2 durch F‐‐Addition (A) dargestellte Titelverbindung (I) wird durch Einengen der SO2‐Lösung in Form farbloser Einkristalle abgeschieden (rasche Dunkelfärbung durch Hydrolyse bzw. Zersetzung).
Nucleophile Substitutionen an Thiazylfluorid (NSF) sollten den Zugang zu Thiazylderivaten R—SN eröffnen. Bei der Reaktion mit LiOCMe3 ließ sich nun erstmals das Primärprodukt „LiNS(F)OCMe3”︁ als Doppelcluster 1 abfangen und durch Röntgen‐Strukturanalyse charakterisieren. Wesentlich für die Entstehung von 1 ist das Molverhältnis NSF : Nucleophil < 1 : 1.magnified image
The preparation of S4N5F by fluoride ion addition to the S4N5 +-cation in liquid SO2 is described. The structure of the fluoride was determined from single crystal data. The mechanism for the formation of S4N5F and the stability of possible isomers is discussed on the basis of MNDO/1 calculations
Die Darstellung der Titelverbindung (IIIa) kann einmal durch Zers. des Hexafluoroarsenats (I) in SO2 (keine Ausb.-Angaben) oder durch Cl"- Austausch in S4N5Cl(VI)mit AgAsF6(VII)in SO, erfolgen.
Abstract N2S3Cl+ SbCl6- was prepared by chlorination of N4S4 · SbCls5 with elemental chlorine. The crystals are monoclinic, P21/c, with a = 1492.4(4), b = 1233.6(2), c = 1437.5(4) pm, β = 91.40(2)°, and R = 0.059 for 3663 observed reflections. There are two independent cations and anions in the asymmetric symmetric unit. The appreciable interionic interaction results in a high density of ρ = 2.642 g · cm -3 (calcd).
The reaction of 1,1-diphenylhydrazine with S2Cl2 in the presence of triethylamine leads to 1,1-diphenylthionitrosamine. The chromium pentacarbonyl derivative was isolated and characterised by X-ray structure determination; [Cr(SNNPh2)(CO)5](2) crystallises in the space group P21/c with a= 786.5(1), b= 2 236.5(2), c= 1 054.6(1) pm, β= 89.44(8)°, and Z= 4; [Cr(SNNMe2)(CO)5](3) also crystallises in P21/c, with a= 1 042.2(3), b= 1 250.7(4), c= 954.6(3) pm, β= 110.21(3)°, and Z= 4. The structures were refined to R= 0.079 for 1 573 diffractometer data with F > 3σ(F), and R= 0.049 for 2 388 data with F > 3σ(F) respectively. The structures are similar, with CrSNNC2 planes approximately eclipsed to the carbonyls. One of the phenyl groups in (2) can take part in π interaction with the nitrogen atoms, which is associated with longer N–N and shorter S–N and Cr–S bonds in (2) than in (3).
AbstractDie gemäß Reaktion A dargestellte Titelverbindung kristallisiert in der Raumgruppe P21/c. In der asymm. Einheit liegen 2 unabhängige Kationen und Anionen vor.
Preparation de S 4 N 5 F par addition de F − au cation S 4 N 5 + dans SO 2 liquide. Etude RX de la structure. Mecanisme de la formation
AbstractAus den Komponenten Dicyan (I) und C1, entsteht in Gegenwart von HgFz unter Ausschluß von Feuchtigkeit nach 4‐tägigem 4 Stehen bei Zimmertemperatur (RT) und 48 h bei 150°C ein Gemisch der Produkte (IIa)‐(IVa).
Die Titelverbindungen XNCFCFNX (13, 14, X = Cl, Br) lassen sich in einfacher Weise aus den drei Komponenten Dicyan, X2 und HgF2 gewinnen. Als weitere Produkte konnten die N-halogenierten Amino- bzw. Iminoperfluorethane Cl2NCF2CF2NCl2 (11), ClNCF-CF2NCl2 (12), BrNCFCF2NBr2 (15) und Br2NCF2CF2NBr2 (16) nachgewiesen werden. Aus Einkristall-Röntgenbeugungsdaten wurde die Struktur von 14 bestimmt. N,N′-Dihalogenoethanediirnidoyl Difluorides The title compounds XNCFCFNX (13, 14, X = Cl, Br) are prepared in a simple way from the three components (CN)2, X2, and HgF2. The N-halogenated amino- or iminoperfluoroethanes Cl2NCF2CF2NCl2 (11), ClNCFCF2NCl2 (12), BrNCFCF2NBr2 (15) and Br2NCF2CF2NBr2 (16) were identified as further products. The structure of 14 was determined from single-crystal X-ray data.
The preparation of S4N5 + MF6- (5 a, b M = As, Sb) by decomposition of S3N3F2 + MF6- and by Cl- exchange in S4N5Cl with AgAsF6 is described. The structure of 5a was determined from single crystal X-ray data.