X-ray diffraction and solid-state [sup.119]Sn CP-MAS NMR studies of some triaryltin(IV) chlorides

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From: Canadian Journal of Chemistry(Vol. 81, Issue 11)
Publisher: NRC Research Press
Document Type: Author abstract
Length: 187 words

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Abstract :

The solid-state [sup.1l9]Sn cross-polarization (CP) magic angle spinning (MAS) NMR spectra of a series of triaryltin chlorides of the form [Ar.sub.3]SnCl have been acquired. The indirect spin-spin coupling constants (J([sup.119]Sn-[sup.35]Cl)), quadrupolar-dipolar shifts (d([sup.l19]Sn-[sup.35]Cl)), and the [sup.1l9]Sn chemical shift tensors were extracted. For the spectrum of triphenyltin chloride (I) the validity of the first-order perturbation approximation was tested by comparing results of both the perturbation and cubic-equation approaches and a variable-temperature NMR study undertaken to investigate the influence of the previously reported molecular motion in the solid. The X-ray crystal structures of the tris(otolyl)tin chloride (II) and tris(p-tolyl)tin chloride (IV) complexes have been examined. They belong to the monoclinic and triclinic space groups [P2.sub.1]/n and P[bar]1, respectively, which are different from the previously reported tris(m-tolyl)tin chloride (III) complex, which crystallizes in the space group R3 and has threefold molecular symmetry. The structures and NMR properties of the complexes with meta-substituents are quite different from those with ortho- or parasubstituents having axially symmetric shift tensors with small spans and larger J values. Key words: aryltin chlorides, magic angle spinning NMR, tin-chlorine spin-spin coupling, [sup.119]Sn chemical shift tensor, crystal structure.

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Gale Document Number: GALE|A111980856