Mr. Maurya et al., DIOXOTUNGSTEN(VI) COMPLEXES OF ONO DONOR LIGANDS AND THE X-RAY CRYSTAL-STRUCTURE OF [WO2(O-OC6H4CH=NN=C(O)C6H5)(MEOH)]CENTER-DOT-MEOH, Bulletin of the Chemical Society of Japan, 68(10), 1995, pp. 2847-2852
A general method for the preparation of dioxotungsten(VI) complexes of
the type [WO(2)L(MeOH)] (where LH(2)=the Schiff's base derived from s
alicylaldehyde or o-vanillin and benzoylhydrazide, salicylhydrazide, f
uroylhydrazide, and isonicotinoylhydrazide) using [WO2(acac)(2)] (acac
H=acetylacetone) as a precursor, is described. These complexes have be
en characterized by elemental analysis, electrical conductance, IR, el
ectronic, and NMR spectral, electrochemical, and magnetic susceptibili
ty measurements. The structure of [WO2(o-C6H4CH=NN=C(O)C6H5) (MeOH)].
MeOH (1a . MeOH) has been determined by single-crystal X-ray diffracti
on analysis. 1a . MeOH crystallizes in the space group Pbc2(1) with a=
6.992(2), b=16.190(2), c=31.390(4) Angstrom, V=3553.4(12) Angstrom(3),
Z=8, R(F)=0.050, and R(w)=0.054. The tungsten atom has a highly disto
rted octahedral coordination in which anionic oxygen atoms of the trid
entate ligand are mutually trans and are cis to the cis-dioxo group.