200336-53-4Relevant articles and documents
Some further studies of estertin compounds. Crystal structures of [NEt4][MeO2CCH2CH2Sn(dmio) 2] (dmio = 1,3-dithiole-2-one-4,5-dithiolato) and (MeO2CCH2CH2)2SnX2[X 2 = I2, (NCS)2 or Cl, Br]
Balasubramanian, Revathi,Chohan, Zahid H.,Doidge-Harrison, Solange M. S. V.,Howie, R. Alan,Wardell, James L.
, p. 4283 - 4295 (1997)
Estertin compounds, (MeO2CCH2CH2)2SnX2 [X2 = I2 (2); X2 = Br2 (9); X2 = Cl,Br (4); or X2 = (NCS)2 (3)] have been obtained by halide exchange reactions of (MeO2CCH2CH2)2SnCl2. Crystal structure determinations of 2-4 revealed chelating MeO2CCH2CH2 units with distorted octahedral geometries at tin. The Sn-O bond lengths in the isothiocyanato complex, 3, are shorter [2.390(11) to 2.498(12), mean 2.439 A], with the chelate bite angles, C-Sn-O, larger [74.3(7) to 78.2(6), mean 76.0°] than those in the halide analogues 2 and 4 [Sn-O = 2.519(2) to 2.541(8), mean 2.530 A; C-Sn-O 72.8(3) to 73.9(4), mean 73.3°]. 1H, 13C and 119Sn NMR and IR spectra of 2-4 and 9 were determined in CDCl3 solution: the NMR spectra of (MeO2CCH2CH2)2SnX2 show the following trends: (i) both δ1Hα and δ13Cα, increase and (ii) both 2J(Sn-H) and 1J(Sn-C) decrease in the sequence X2 = (NCS)2, Cl2, ClBr, Br2 and I2. The MeO2CCH2CH2 and dmio groups (dmio = 1,3-dithiole-2-one-4,5-dithiolato) are all chelating groups in (MeO2CCH2CH2)2Sn(dmio) (5). As shown by X-ray crystallography, the tin atom in the anion of solid [Q][MeO2CCH2CH2Sn(dmio)2] 6 (Q = NEt4) forms 5 strong bonds [to C and the 4 thiolato S atoms, Sn-S 2.459(2) to 2.559(2) A], arranged in a near trigonal bipyramidal array. There is an additional intramolecular, but weaker, interaction with the carbonyl oxygen atom [Sn-O = 3.111(5) A]; v(C=O) = 1714 cm-1 in solid 6 (Q = NEt4). NMR spectra of 5 and 6 are also reported.
