Synthesis and Spectroscopic Investigations of Some Binuclear Organotin(IV) Complexes of Malonobis(salicylidenehydrazide) and Crystal Structure Study of 22CH2

Article abstract of DOI:10.1246/bcsj.67.1797

The Schiff base, 2CH2 , derived from the condensation of salicylaldehyde and malonodihydrazide, reacted with organotin chlorides to yield binuclear complexes of the type R2SnSnR2, where R=CH3-, C2H5-, C4H9-, C6H5-, CH3CO2CH2CH2-, and C6H5CH2-.The complexes were characterized and the structure assigned on the basis of their elemental analysis, IR, 1H, 13C, 119Sn NMR spectral, and X-ray crystallographic data.In these complexes, the ligand functions as a flexibly bridging tetrabasic hexadentate moiety binding two tin atoms through ONO donor atomsand both tin atoms are in trigonal bipyramidal environment.A single crystal diffraction study of the complex, <(C2H5)2Sn>2(OC6H4CH=NNCO)2CH2, confirms the structure to be binuclear.The crystals are monoclinic, space group I2/a with a=12.312(2), b=11.526(2), c=18.858(2) Angstroem, β=94.69(2) deg, volume=2667.1(7) Angstroem³, 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 bridged to the other half by two fold symmetry via C(13) atom.The tin atom has distorted trigonal bipyramidal coordination with two oxygens occupying axial positions while two ethyl groups and azomethine nitrogen occupy the equatorial positions.The two ethyl groups coordinated to tin are cis to each other.