Four known dithiophosphinic acids, DTPA, were synthesized and their zinc complexes were newly prepared. The complexes have been proven to have the structures [Zn(µ-DTPA n )2(DTPA n )2], ([DTPA n ]= R n (R)P(S)H, R= 4-CH3O-C6H4-; R 1 = iso-amyl-, DTPA 1 ; R 2 = iso-butyl-, DTPA 2 ; R 3 = sec-butyl-, DTPA 3 ; R 4 = iso-propyl-, DTPA 4 ). The DTPAs were prepared by the reaction of the Lawesson reagent, [2,4-bis(4-methoxyphenyl)-1,3,2,4-dithiodiphosphetane-2,4-disulfide] (LR), with the corresponding Grignard compounds. The acids formed are viscous liquids difficult to purify and so they were converted to ammonium salts, [DTPA n ][NH4], which are easy to obtain as pure crystals. The complexes were identified to have dimeric structures on the basis of mass spectroscopic data. Cite this: Sağlam E, Acar N. Syntheses and characterization of new dithiophosphinato zinc complexes. JOTCSA. 2018;5(2):931-40.