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A study of the mode of coordination in the complexes of a number of nitrogen and sulfur containing ligands with Co(II) and Ni(II) ions has been made, based on the i.r. data of the shifts in the thioamide bands I, II, III and IV in the ligands on complexation. The ligands are 1-substituted tetrazoline-5-thiones (1ST5TH), 3-(4-pyridyl)triazoline-5-thione (3, 4PT5TH) thiazolidine-2-thione (tt) and thiocarbohydrazide (Htcaz). A number of complexes Co(1-ST5T)₂, Ni(1ST5T)₂, Co(tt)₂Cl₂, Ni(tt)₂I₂, Co(3, 4PT5T)₂-Py₂, M(Htcaz)₂X₂ (where X = CNS, Cl, Br, I, NO₃ and M = Co(II), Ni(II), and Co(Htcaz)₂SO₄. 3H₂O, have been prepared.