SYNTHESIS AND CHARACTERIZATION OF TRIPHENYLTIN AND TRI-N-BUTYLTIN PENTAFLUOROBENZOATES, PENTAPHENYLACETATES AND PENTACINNAMATES - X-RAY STRUCTURE DETERMINATION OF TRI-N-BUTYLTIN PENTAFLUOROCINNAMATE
R. Willem et al., SYNTHESIS AND CHARACTERIZATION OF TRIPHENYLTIN AND TRI-N-BUTYLTIN PENTAFLUOROBENZOATES, PENTAPHENYLACETATES AND PENTACINNAMATES - X-RAY STRUCTURE DETERMINATION OF TRI-N-BUTYLTIN PENTAFLUOROCINNAMATE, Journal of organometallic chemistry, 514(1-2), 1996, pp. 203-212
A crystal structure analysis of F5C6-CH = CH-COOSnBu(3) shows that the
compound is polymeric because of the presence of bidentate carboxylat
e ligands bridging two tin atoms in trans-R(3)SnO(2) arrangement. This
results in a five-coordinated trigonal-bipyramidal geometry around th
e tin atom with two apical oxygen atoms and three equatorial butyl gro
ups. Mossbauer and CP-MAS Sn-117 NMR data for triphenyl- and tri-n-but
yltin pentafluorobenzoates, -phenylacetates and cinnamates, taking the
X-ray structure ofF(5)C(6)-CH=CH-COOSnBu(3) as a reference, converge
to similar polymeric five-coordinated structures in the solid state. I
n contrast, C-13 Sn-119 NMR data in chloroform solution unambiguously
indicate tetrahedral four-coordination at tin for all compounds. Faili
ng and C-13 chemical shift increments and complex (n)J(C-13-F-19) mult
iplet patterns necessitated recording of 2D F-19-C-13 HMQC spectra aro
matic in order to fully characterize the new compounds in solution.