ISSN:
0749-1581
Keywords:
Determination of coupling signs
;
Multinuclear two-dimensional NMR
;
Pseudo-triple-resonance experiments
;
Solid-state
;
119Sn CP/MAS NMR
;
Cyclopentadienyltin(II) compounds
;
Chemistry
;
Analytical Chemistry and Spectroscopy
Source:
Wiley InterScience Backfile Collection 1832-2000
Topics:
Chemistry and Pharmacology
Notes:
Absolute coupling signs of 1J(119Sn, 13C) (〈O) and 2J(119Sn, 1H) (〈O) in (n5-C5H5)2Sn (1) and 1J(119Sn, 13C) (〈O)2J(119Sn, 13C) (〈O) and 3J(119Sn, 1H) (〉O) in (n5-C5Me5)2Sn (2) were determined using advanced direct and indirect two-dimensional methods. These are based on Ψ-BIRD techniques and z-filtering, leading to pseudotriple-resonance experiments of the type 1H{119Sn(13C)} and 13C{1H(119Sn)}, respectively. A mixed n5-cyclopentadienyltin(II) amide was prepared and characterized by 1H, 13C, 29Si and 119Sn NMR in solution in the presence of its symmetrical redistribution products 1 and [(Me3Si)2N]2Sn. Solid-state 119Sn CP/MAS NMR spectra of 1 shows the presence of two tin sites (in accord with the x-ray analysis) with a 62.2 ppm difference in 119Sn chemical shifts, the mean value being in close agreement with the solution-state δ119Sn value. The symmetries of the shielding tensor for the two tin sites are different and there appears to be a correlation between this property and the ring centroid - Sn - ring centroid angle α. 13C CP/MAS NMR proved insensitive to the structural differences between the two types of molecules of 1 in the unit cell.
Additional Material:
3 Ill.
Type of Medium:
Electronic Resource
URL:
http://dx.doi.org/10.1002/mrc.1260301010
Permalink
