18156-25-7Relevant articles and documents
Nitrogen NMR of Some Sulphur Diimide Anions and Calculated (GIAO) Nitrogen Shielding Constants
Wrackmeyer, Bernd,Gerstmann, Silke,Herberhold, Max,Webb, Graham A.,Kurosu, Hiromichi
, p. 492 - 495 (1994)
Sulphur diimide anions of the type (2-) (1), (-) (1), were prepared with the counter ions (+) or (+) (for 1, 3, 4) and K(+) (for 5) and studied in solution by 14N NMR, and for assignment purposes by 15N NMR (4).The experimentally determined 14N chemical shifts (δN) were compared with nitrogen shielding constants calculated by the gauge included atomic orbitals (GIAO) technique, and a linear relationship between ?N(calc) and δN was obtained.This correlation serves to support the Z configuration of the anions (-), analogous to the isoelectronic N-sulphinylamines.On the basis, two 14N resonance signals reported in the literature with uncertain assignment can be attributed to (-) (2), and the previously assigned δN values suggest that the anion (-) (6) adopts the Z/E configuration. - Keywords: Sulphur diimide anions Configuration 14N NMR 15N NMR Nitrogen shielding GIAO calculation
Gas-phase Molecular Structure of N,N'-Bis(trimethylsilyl)sulphur Di-imide, determined by Electron Diffraction
Anderson, David G.,Robertson, Heather E.,Rankin, D. W. H.,Woollins, J. Derek
, p. 859 - 862 (1989)
The molecular geometry of Me3SiNSNSiMe3 in the gas phase has been studied by electron diffraction.The molecule has C2 symmetry with a distorted syn,syn conformation.Principal parameters are : ra(S=N) 153.6(3), ra(Si-N) 173.8(3), and ra(Si-C) 186.9(1) pm; NSN 129.5(16), SNSi 132.9(7), and SN twist (relative to syn,syn conformation) 42(1) deg.
Solid-state Structure of Sulfur Bis(trimethylsilylimide), S(NSiMe3)2, and Multinuclear Magnetic Resonance Studies of Some Sulfur Bis(silylimides) in Solution
Herberhold, Max,Gerstmann, Silke,Wrackmeyer, Bernd,Borrmann, Horst
, p. 633 - 636 (1994)
In the solid state sulfur bis(trimethylsilylimide) 1 has been shown to adopt the E/Z configuration by single-crystal X-ray diffraction (space group P, triclinic).In solution sulfur bis(silylimides) R(NSN)R' are fluxional at room temperature.Comparison of the 1H, 13C, 29Si and, in particular, 15N NMR data indicates that 1 and 2 undergo rapid E/Z Z/E isomerization even at 173 K, whereas in the case of 3 and 4 this process is slowed at low temperature and the E/Z configuration prevails with the SiMe3 group in the E position.
Cyclic Sulfur Diimides of Silicon. (15)N NMR Spectroscopy and the X-Ray Analysis of the Eight-Membered Ring tBu2Si(NSN)2SitBu2
Herberhold, Max,Gerstmann, Silke,Milius, Wolfgang,Wrackmeyer, Bernd
, p. 1041 - 1050 (2007/10/02)
Various six-membered cyclic sulfur diimides (3a-f) were prepared by aminolysis of the bis(chloro-dimethylsilyl)sulfur diimide (2) using NH3 (a) and primary amines RNH2 nPr (d), nBu (e), iPr (f)>.Except for R = H, non-cyclic intermediates, the Si-monoamino- (7) and Si,Si'-diamino derivatives of 2 (8), were detected for all groups R, including R = tBu (g).The reaction between R2SiCl2 and the sulfur diimide anion K gave non-cyclic silanes (9,10) and the eight-membered rings of the type R2Si(NSN)2SiR2 tBu (5)> of which 5 was studied by X-ray analysis (monoclinic, space group P21/c; planar ring system) and solid-state (15)N and (29)Si CP/MAS NMR spectroscopy.The ten-membered ring system 6 was obtained from the reaction between 1,2-dichloro-tetramethyldisilane and bis(trimethylstannyl)sulfur diimide.All compounds were studied by (1)H, (13)C, (15)N and (29)Si NMR.The δ(15)N NMR data proved useful to distinguish between fluxional systems with fast E/Z-Z/E isomerization (non-cyclic compounds 8 and the ten-membered cycle 6).Hahn-Echo-extended (HEED) polarization transfer (INEPT) pulse sequences served to measure coupling constants 1J((29)Si(15)Namine) for the compounds 3 and 8.This also proved that the magnitude of 1J((29)Si(15)NNSN) must be small (1J((29)Si(15)Namine) and 1J((15)N(1)H) (3a) indicated that the amino-nitrogen atom adopts a pyramidal environment.
