Several complexes of the type, [M{S₂CNR}₃](1)(M=Ga or In;R=CH₂CH₂OCH₂CH₂, CH₂CH₂N(Me)CH₂CH₂),[MCl₂{S₂CN(CH₂CH₂)₂O}](2) (M=Ga or In), [MCl{S₂CN(CH₂CH₂)₂O}₂](3) (M=Ga or In),[Ga{S₂CN(CH₂-CH₂)₂O}{S₂P(OR)₂}₂](4) (R=Et, Prⁱ) and [M{S₂CNR}{(SCH₂CH₂)₂O}] (5) (M=Ga or In; R=CH₂CH₂OCH₂CH₂,CH₂CH₂N(Me)CH₂CH₂) ave been prepared. All the complexes were characterized by elemental analysis, IR and NMR (¹H,¹³C{¹H}) spectroscopy.⁷¹Ga NMR chemical shifts and half line widths are influenced by the coordination number of gallium and the substituents on the ligand moiety. Single crystal X-ray structures of two complexes [M{S₂CN(CH₂CH₂)₂O}₃] (M=Ga, In)have been determined.