Infrared, Sn-119, C-13 and H-1 NMR, Sn-119 and C-13 CP/MAS NMR and Mossbauer spectral study of some tributylstannyl citrates and propane-1,2,3-tricarboxylates
J. Holecek et al., Infrared, Sn-119, C-13 and H-1 NMR, Sn-119 and C-13 CP/MAS NMR and Mossbauer spectral study of some tributylstannyl citrates and propane-1,2,3-tricarboxylates, COLL CZECH, 64(6), 1999, pp. 1028-1048
Citations number
25
Categorie Soggetti
Chemistry
Journal title
COLLECTION OF CZECHOSLOVAK CHEMICAL COMMUNICATIONS
Six tributylstannyl citrates and three tributylstannyl propane-1,2,3-tricar
boxylates of the formula (RC)-C-1(CH2COOR2)(COOR3)(CH2COOR4) (R-1 = OH or H
, R-2, R-3, R-4 = H, Bu3Sn, C6H11NH3, (C6H11)(2)NH2 or (CH2)(5)NH2) have be
en synthesised, and their solution and solid-state structures studied by in
frared, H-1,C-13 and Sn-119 NMR, C-13 and Sn-119 CP/MAS NMR and Sn-119 Moss
bauer spectroscopies. In non-coordinating solvents, the compounds exist as
isolated molecules or ionic-pairs with their tin atoms in pseudotetrahedral
environments. In coordinating solvents, the tin atoms in the compounds are
five-coordinate owing to the participation of the solvent in bonding; and
their trans-trigonal bipyramidal coordination spheres consist of the ipso-c
arbon atoms of the butyl substituents in equatorial plane, and the solvent
molecule and the oxygen atom of the monodentate carboxyl group in axial pos
itions. A part of tributylstannyl groups together with some bidentate bridg
ing carboxylate groups form polymeric chains in the solid state of citrates
and propane-1,2,3-tricarboxylates. Also dioxastanna-rings with the partici
pation alpha-hydroxycarboxylate fragments and one of the tributylstannyl gr
oups occur probably in some citrates in the solid state. The spectroscopic
assignment for the citrate has been confirmed by crystal structure analysis
. Key words: Stannanes; Organotin compounds; Citrates; Propane-1,2,3-tricar
boxylates; IR spectroscopy; NMR spectroscopy,H-1, C-13 and Sn-119; CP/MAS N
MR spectroscopy,C-13 and Sn-119; Mossbauer spectroscopy; Crystal structure.