New Ni(II)-organophosphonate species were synthesized in aqueous solution under specific conditions. Glyphosate, N-(phosphonomethyl) glycine and imino bis(methylphosphonic acid), H2O3P-CH2-NH2+-CH2-PO3H-, interacted with Ni(II) and the pH was adjusted with addition of ammonia and other bases. Each isolated crystalline product was isolated and was characterized by elemental analysis, spectroscopic techniques (FT-IR), and X-ray crystallography.