Several complexes of the type, [M{S 2 CNR} 3 ] (1) (M=Ga or In; R=CH 2 CH 2 OCH 2 CH 2 , CH 2 CH 2 N(Me)CH 2 CH 2 ), [MCl 2 {S 2 CN(CH 2 CH 2 ) 2 O}] (2) (M=Ga or In), [MCl{S 2 CN(CH 2 CH 2 ) 2 O} 2 ] (3) (M=Ga or In), [Ga{S 2 CN(CH 2 CH 2 ) 2 O}{S 2 P(OR) 2 } 2 ] (4) (R=Et, Pr i ) and [M{S 2 CNR}{(SCH 2 CH 2 ) 2 O}] (5) (M=Ga or In; R=CH 2 CH 2 OCH 2 CH 2 , CH 2 CH 2 N(Me)CH 2 CH 2 ) have been prepared. All the complexes were characterized by elemental analysis, IR and NMR ( 1 H, 1 3 C{ 1 H}) spectroscopy. 7 1 Ga 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{S 2 CN(CH 2 CH 2 ) 2 O} 3 ] (M=Ga, In) have been determined.