Abstract
High-resolution NMR spectra of spin- 1 2 nuclei, particularly 119Sn and 31P, in solid tin(II) phosphite, SnHPO 3, and tin(II) phosphate, SnHPO 4, are presented. The results are discussed in relation to the crystal structures. Spinning sideband analysis has been carried out for both nuclei, giving information on the shielding tensors. Satellite peaks allow the indirect Sn,Sn coupling constants to be determined. Surprisingly large values of 2600±200 Hz and 4150±200 Hz are reported for SnHPO 3 and SnHPO 4 respectively. The satellite peaks were investigated by using a single Hahn echo for each refocusing time, which showed that the observed splittings result from 119Sn, 117Sn coupling. For SnHPO 3, the calculated relative intensities of the satellites for six intra-layer coupling interactions are in agreement with the experiment values, but for SnHPO 4 the coupling appears to be inter-layer in nature. Tin-119 (and in one case phosphorus-31) shielding tensor data derived from MAS NMR are also reported for four other crystalline tin(II) compounds, namely tin diphosphate, tin oxalate, tin sulphate and calcium tin ethylenediamine tetraacetate.
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