A. Mazouz et al., TETRASELENA CROWN-ETHERS - SYNTHESIS AND COMPLEXATION WITH MERCURY SALTS - CRYSTAL-STRUCTURE OF A MACROCYCLE AND A MERCURY(II) COMPLEX, Journal of the Chemical Society. Dalton transactions, (6), 1997, pp. 1043-1048
Dipotassium benzene-1,2-diselenolate, C6H4(SeK)(2)-1,2 obtained from t
he reaction of potassium tert-butoxide with a (benzene-1,2-diselenolat
o)zirconocene, was treated with C6H4[SeCH2(CH2OCH2)(n)CH(2)X](2)-1,2 (
X = Cl, n = 11, n = 22, n = 33 or X = Pr n = 34) leading to tetraselen
acrown ethers C6H4[SeCH2(CH2OCH2)(n)CH2Se](2)- C6H4 (n = 16, n = 27 or
n = 38) in a moderate yield (10-20%). This yield can be increased by
using the 'caesium effect' from benzene-1,2-diselenol (18-40%). These
macrocyclic compounds are able to complex heavy metals [especially mer
cury(II) ions] via their selenium atoms. The mercury complexes have be
en characterized by multinuclear NMR spectroscopy. The molecular struc
tures of the tetraselenacrown ether 7 and the mercury complex of macro
cycle 8 have been established by X-ray diffraction.