AbstractThe reaction between bis(1,2,3‐triazol‐1‐yl)methane derivatives and ⁿBuLi and various aldehydes, yielded novel neutral ligand precursors incorporating alcohol functional groups. The resulting compounds exhibited distinct characteristics depending on the steric hindrance of the aldehyde employed. In instances where aromatic aldehydes were utilized, functionalization occurred at the methine group bridging both triazole rings. Conversely, the use of pivalic aldehyde prompted functionalization at the C⁵ position of the triazole ring. These compounds were subsequently employed as ligand precursors in the synthesis of organometallic aluminum and zinc complexes, yielding dinuclear complexes with high efficiency. The structural elucidation of all compounds was accomplished through spectroscopic methods and validated by X‐ray crystallography. Preliminary catalytic investigations into the coupling reaction of cyclohexene oxide and CO₂ revealed that aluminum and zinc complexes catalyzed the selective formation of polyether and polycarbonate materials, respectively.