Solid-state 119Sn CP/MAS NMR spectra have been obtained for four triorganyltin halides and seven diorganyltin dihalides. The solution-to-solid chemical shift changes are discussed in terms of the solid-state structures and, in the case of benzyl compounds, conformations. Unsymmetrical splittings in some of the spectra are explained as arising from residual dipolar and/or indirect coupling interactions between 119Sn and 35C1, and the results are the first reported examples of this type. Some tin-119 CP/MAS results of general significance on other compounds are mentioned for the purpose of comparison.

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Benzyltrialkyl-(1-13) and benzyltriphenylstannanes (16)(17)(18)(19)(20)(21)(22) have been easily prepared in a one-pot synthesis via coupling reaction of benzyl bromide derivatives (C 6 H 5 CH 2 Br andPr, Bu, and Ph) in THF/H 2 O (NH 4 Cl) medium mediated by zinc powder. Such coupling also occurs with (Bu 3 Sn) 2 O. Dibenzyldibutylstannane (15) is prepared by reaction of benzyl bromide with Bu 2 SnCl 2 or (Bu 2 SnCl) 2 O, and (2-naphthylmethyl)tributylstannane (14) by reaction of 2-(bromomethyl)naphthalene with Bu 3 SnCl. 13 Cand 119 Sn-NMR data are reported for all compounds, and Mo ¨ssbauer data for benzyltributylstannanes 10 and 11 and benzyltriphenylstannanes 16-18 and 20-22. The crystal structures of Ph 3 SnBn, with Bn ) o-(17) and m-ClC 6 H 4 CH 2 (18) and o-(20) and m-FC 6 H 4 -CH 2 (21) have been determined.

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