Solid-state NMR studies of some tin(II) compounds |
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Authors: | Amornsakchai Pornsawan Apperley David C Harris Robin K Hodgkinson Paul Waterfield Philip C |
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Affiliation: | a Department of Chemistry, University of Durham, South Road, Durham DH1 3LE, UK b Unilever Research (Port Sunlight Laboratory), Quarry Road East, Bebington, Wirral L63 3JW, UK |
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Abstract: | High-resolution NMR spectra of [Formula: see text] nuclei, particularly (119)Sn and (31)P, 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+/-200Hz and 4150+/-200Hz 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 (119)Sn, (117)Sn 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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Keywords: | Solid-state NMR Tin (II) Shielding tensors Sn,Sn coupling Spinning sidebands Layer structures. |
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