The tri-n-butyltin(IV) complexes of 2-[(E)-2-(3-formyl-4-hydroxyphenyl)-1-diazenyl]benzoic acid and 4-[((E)-1-{2-hydroxy-5-[(E)-2-(2-carboxyphenyl)-1-diazenyl]phenyl}methylidene)amino]aryls (aryls = 4-CH 3 , 4-Br, 4-Cl, 4-OCH 3 ) have been synthesized and characterized by 1 H, 13 C, 119 Sn NMR, IR and 119m Sn Mö ssbauer spectroscopic techniques in combination with elemental analysis. The crystal structures of two compounds, (Bu 3 Sn[O 2 CC 6 H 4 {N@N(C 6 H 3 -4-OH-5-CHO)}-o]) n and (Bu 3 Sn[O 2 CC 6 H 4 -{N@N(C 6 H 3 -4-OH(C(H)@NC 6 H 4 Cl-4))}-o]) n , are reported.The crystallographic and 119 Sn Mö ssbauer data both indicate that the tributyltin complexes form single-stranded polymeric structures in which the carboxylate O atoms of each aryl ligand bridge two Sn atoms. The Sn atoms have a slighly distorted trigonal bipyramidal coordination geometry with equatorial butyl groups and carboxylate O atoms occupying axial positions. The 119 Sn NMR spectroscopic data and the 1 J( 13 C-119/117 Sn) coupling constant indicate a tetrahedral coordination geometry in non-coordinating solvents. The results of a toxicity study of a tributyltin compound on the second larval instar of Aedes aegypti mosquito larvae are reported.