The water soluble ligands, lithium and potassium tris(3-isopropylpyrazol-1-yl)methanesulfonate (LiTpms i Pr and KTpms i Pr) and potassium hydrotris(3-carboxyethyl-5-methylpyrazol-1-yl)borate (), have been prepared and their reactions with simple Mo-containing starting material investigated. The crystal structure of LiTpms i Pr·1.2MeOH consists of dinuclear units containing two distinctly different, four-coordinate, tetrahedral Li centers coordinated by bidentate κ2 N,O-Tpms i Pr− and methanol. The ligands fail to coordinate to aqueous molybdate under neutral to acidic conditions. Reaction of with MoO2Cl2(OPPh3)2 results in reduction and formation of MoVOCl3(OPPh3)2·MoVIO2Cl2(OPPh3)2. The crystal structure of this binary mixture revealed distorted octahedral molecules in crystallographically distinct sites.