A new pyrazole containing ligand, 5-methyl-3-formylpyrazole-N(4)-dihexylthiosemicarbazone (HMPzNHex2), and a host of its cobalt(III) and nickel(II) complexes, [Co(MPzNHex2)2]X·mH2O and [Ni(HMPzNHex2)2]X2·nH2O (X= Cl, Br, ClO4, BF4 and NO3; m = 0 for Cl, Br, BF4 & NO3 and 1.5 for ClO4; n = 0 for Br, ClO4, BF4 & NO3 and 2 for Cl), respectively, have been synthesized and characterized by elemental analyses, magnetic measurements (polycrystalline state), 1 H NMR (for the ligand and its Co(III) complexes), electronic and IR spectral parameters. All the reported Co (III) and Ni(II) complexes are cationic in nature and behaving as 1:1 and 1:2 electrolytes, respectively, in MeOH. Electronic spectral data of the complexes categorize them as having distorted octahedral coordination geometry. IR spectral features (4000-/450 cm -1 ) specify a monodeprotonated / neutral tridentate (NNS) function of the ligand, HMPzNHex2 coordinating to the Co(III) / Ni(II) via the pyrazolyl (tertiary) ring nitrogen, azomethine nitrogen and thiolato / thioketo sulfur atom. 1 H NMR spectral data (in CDCl3 at 400 MHz) for the primary ligand and those of its Co(III) complexes are in agreement with the proposition of bonding sites evidenced from IR data. The single crystal x-ray data of I (C2/c (#15); monoclinic) and II (P-1 (#2); triclinic) have confirmed a CoN4S2 and a NiN4S2 octahedral coordination, respectively. The pair of monoprotic / neutral coordinating ligands