A series of organotin(IV) complexes of composition R 3 Sn[O 2 CC 6 H 4 {N= C(H)C 6 H 3 -2-OH(N=NC 6 H 4 R)}-p] (R = Ph or Bz; R = H, 2-CH 3 , 3-CH 3 , 4-CH 3 ) have been investigated by 119 Sn Mössbauer, 1 H, 13 C, 119 Sn NMR and IR spectroscopic techniques. 119 Sn Mössbauer data indicated a distorted tetrahedral geometry for the triphenyltin(IV) complexes while the tribenzyltin complexes exhibit a distorted trigonal bipyramidal coordination geometry with equatorial benzyl groups and the axial positions occupied by an O atom from the carboxylate ligand and the O atom from the water ligand. The 119 Sn-NMR chemical shifts confirm that the Sn atom in triorganotin complexes is four-coordinate in CDCl 3 solution.