PREPARATIONS AND CRYSTAL-STRUCTURES OF SN(CH(2)CH(2)CO(2)ME)(2)(C3S5)AND [Q][SN(CH(2)CH(2)CO(2)ME)(C3S5)(2)] (Q=NET(4) OR 1,4-DIMETHYLPYRIDINIUM, C3S5=4,5-DISULFANYL-1,3-DITHIOLE-2-THIONATE)
H. Buchanan et al., PREPARATIONS AND CRYSTAL-STRUCTURES OF SN(CH(2)CH(2)CO(2)ME)(2)(C3S5)AND [Q][SN(CH(2)CH(2)CO(2)ME)(C3S5)(2)] (Q=NET(4) OR 1,4-DIMETHYLPYRIDINIUM, C3S5=4,5-DISULFANYL-1,3-DITHIOLE-2-THIONATE), Journal of the Chemical Society. Dalton transactions, (4), 1996, pp. 541-548
The compounds Sn(CH(2)CH(2)CO(2)Me)(2)(C3S5) 1 (R = Me or Pr-1) and [Q
][Sn(CH(2)CH(2)CO(2)Me)(C3S5)(2)] 2 (Q = NEt(4) or 1,4-dimethylpyridin
ium; C3S5 = 4,5-disulfanyl-1,3-dithiole-2-thionate) have been prepared
and characterised by solution and solid-state NMR spectroscopy. A cry
stal structure determination of 1 (R = Me) revealed it to be a monomer
ic six-co-ordinate, distorted-octahedral complex with chelating MeO(2)
CCH(2)CH(2) groups and trans-carbon atoms [Sn-O(C) 2.629(7) Angstrom].
The MeO(2)CCH(2)CH(2) group in 2, both in solution and in the crystal
, is monodentate: the tin centres in the anions of both complexes 2 we
re shown to have structures closer to rectangular pyramids than to tri
gonal bipyramids. There were, however, slight differences in the solid
-state structures of the anions, particularly in regard to the separat
ions of the Sn and carbonyl oxygen atoms; Sn ... O intramolecular dist
ances are 4.84(1) and 3.371(4) Angstrom in 2 (Q = NEt(4)) and 2 (Q = 1
,4-dimethylpyridinium) respectively. There were also differences in th
e packing of the anions.