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

Citation
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
ISSN journal
00100765 → ACNP
Volume
64
Issue
6
Year of publication
1999
Pages
1028 - 1048
Database
ISI
SICI code
0010-0765(199906)64:6<1028:ISCAHN>2.0.ZU;2-E
Abstract
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.