This research concerns the synthesis of two O-carboxymethyl chitosan (O-CMCs) complexes with Cu(II) and Ni(II). The synthesized complexes were characterized using (FT-IR), UV-visible, and molar conductivity. It is proposed that [Cu(CMCs)2] possess a square planar structure. Whereas [Ni(CMCS)2] supposing that the structure of this complexes is tetrahedral.