Abstract: | The reaction of 4‐mercaptophenylacetic acid with dimethyltin dichloride in the presence of sodium ethoxide in ethanol affords a novel two‐dimensional organotin network structure compound 1, which is an unusual network containing dinuclear 18‐membered and tetranuclear 26‐membered organotin macrocycles. The compound has been characterized by elemental analysis, IR, and 1H, 13C, and 119Sn NMR spectroscopy. Furthermore, we have also characterized the compound by X‐ray crystallography. |