SYNTHESIS OF COMPLEXES OF DIMETHYLTIN(IV) WITH MONO-DEPROTONATED AND DI-DEPROTONATED PYRIDOXINE (PN) IN MEDIA WITH VARIOUS ANIONS - CRYSTAL-STRUCTURES OF [SNME2(PN-H)]NO3-CENTER-DOT-2H(2)O, [SNME2(H2O)(PN-H)]-CL-CENTER-DOT-H2O AND [SNME2(H2O)(PN-2H)]CENTER-DOT-0.5H(2)O
Js. Casas et al., SYNTHESIS OF COMPLEXES OF DIMETHYLTIN(IV) WITH MONO-DEPROTONATED AND DI-DEPROTONATED PYRIDOXINE (PN) IN MEDIA WITH VARIOUS ANIONS - CRYSTAL-STRUCTURES OF [SNME2(PN-H)]NO3-CENTER-DOT-2H(2)O, [SNME2(H2O)(PN-H)]-CL-CENTER-DOT-H2O AND [SNME2(H2O)(PN-2H)]CENTER-DOT-0.5H(2)O, Journal of the Chemical Society. Dalton transactions, (22), 1997, pp. 4421-4430
The reaction of the dimethyltin(IV) cation with pyridoxine [3-hydroxy-
4,5-bis(hydroxymethyl)-2-meth PN] has been investigated in ethanol-wat
er (80:20 v/v) containing NO3- and Cl-, NO3- and MeCO2- or Cl- and MeC
O2- ions in various mole ratios. The compounds [SnMe2(PN-H)]NO3 . 2H(2
)O 1, [SnMe2(H2O)(PN-H)]- H2O 2 and [SnMe2(H2O)(PN-2H)]. 0.5H(2)O 3 we
re isolated and characterized by-IR, Raman, cross polarization magic a
ngle spinning C-13 NMR and electron impact andFAB mass spectrometry. T
he structures of the compounds were determined by X-ray diffraction. I
n I [SnMe2(PN-H)](2)(2+) units in which each moho-deprotonated pyridox
ine co-ordinates to one tin atom via the phenolic O and a deprotonated
CH2OH group O and to the other via the latter group alone are connect
ed in a polymeric structure via the other CH2OH group of each PN-H. In
each dimeric unit the tin atom is co-ordinated to two methyl groups,
the phenolic O atom, the O atoms of two deprotonated CH2OH groups, and
the O atom of a non-deprotonated CH2OH group. Hydrogen-bonded water a
nd NO3- ions are also present in the crystal lattice. In 2 the lattice
contains dimeric [SnMe2(H3O)-(PN -H)](2)(2+) units (in which the tin-
pyridoxine co-ordination is the same as:in 1 except that the bonds con
necting different units in 1 now bind aqua ligands) and hydrogen-bonde
d water and chloride ions. In 3 the crystal contains dimeric [SnMe2(H2
O)(PN-2H)](2) units (in which the dideprotonated ligand co-ordinates a
s in 2) and water. The behaviour of these compounds in D2O and (CD3)(2
)SO was studied by NMR spectroscopy.