SYNTHESIS AND SPECTROSCOPIC INVESTIGATIONS OF SOME BINUCLEAR ORGANOTIN(IV) COMPLEXES OF MALONOBIS(SALICYLIDENEHYDRAZIDE) AND CRYSTAL-STRUCTURE STUDY OF [(C2H5)2SN]2[OC6H4CH=NNCO]2CH2
Mp. Degaonkar et al., SYNTHESIS AND SPECTROSCOPIC INVESTIGATIONS OF SOME BINUCLEAR ORGANOTIN(IV) COMPLEXES OF MALONOBIS(SALICYLIDENEHYDRAZIDE) AND CRYSTAL-STRUCTURE STUDY OF [(C2H5)2SN]2[OC6H4CH=NNCO]2CH2, Bulletin of the Chemical Society of Japan, 67(7), 1994, pp. 1797-1801
The Schiff base, [HOC6H4CH=NNHCO]2CH2 [H4L]. derived from the condensa
tion of salicylaldehyde and malonodihydrazide, reacted with organotin
chlorides to yield binuclear complexes of the type R2Sn[L]SnR2, where
R=CH3-, C2H5-, C4H9-, C6H5-, CH3CO2CH2CH2-, and C6H5CH2-. The complexe
s were characterized and the structure assigned on the basis of their
elemental analysis, IR, H-1, C-13, Sn-119 NMR spectral, and X-ray crys
tallographic data. In these complexes, the ligand functions as a flexi
bly bridging tetrabasic hexadentate moiety binding two tin atoms throu
gh ONO donor atoms and both tin atoms are in trigonal bipyramidal envi
ronment. A single crystal diffraction study of the complex, [(C2H5)2Sn
]2(OC6H4CH=NNCO)2CH2, confirms the structure to be binuclear. The crys
tals are monoclinic, space group I2/a with a=12.312(2), b=11.526(2), c
=18.858(2) angstrom, beta=94.69(2)-degrees, volume=2667.1(7) angstrom3
. Z=4, D(c)=1.718 g cm-3. The final discrepancy factors are R=0.042, R
(w)=0.055 for 1698 observed reflections. Half of the molecule is bridg
ed to the other half by two fold symmetry via C(13) atom. The tin atom
has distorted trigonal bipyramidal coordination with two oxygens occu
pying axial positions while two ethyl groups and azomethine nitrogen o
ccupy the equatorial positions. The two ethyl groups coordinated to ti
n are cis to each other.