Reactions of dithiocarbamates salts (IVa, IVb, IVc) with bis(N‐thiazol) chloroacetamides(IIa, IIb) in DMF furnished corresponding podands as Va, Vb, Vc, Vd, Ve, Vf in high to excellent yields. Two reacting ligands (IIa, IIb) were obtained in the reaction of bis(aminothiazoles) (Ia, Ib) with chloroacetyl chloride. Dynamic NMR spectroscopic data of two series of podands (Va, Vb, Vc and Vd, Ve, Vf) are discussed and figured out their free energy of activation (ΔGc≠) at coalescence temperatures. The ΔGc≠s of these podands were attributed to conformational isomerization in the range of 14.9–16.2 kcal/mol due to rotation and resonance effect about thioamide C―N bond.