Summary: A new chiral rigid bisetherketone macrocycle containing binaphthyl and thioether moieties was synthesized successfully using a modified pseudo‐high dilution technique. The compound was characterized by means of infrared absorption (IR) and vibrational circular dichroism (VCD). The experimental IR and VCD spectra were compared with those computed based on density functional theory (DFT) calculations at B3LYP/6‐31G (d) level. Good agreement was observed between the experimental and calculated spectra and, therefore, the absolute configuration was determined. Knowledge of the absolute configuration is of great importance when exploring the mechanisms of chiral recognition based on the chiral macrocyclic molecules.Structure of the new chiral rigid bisetherketone macrocycle produced.imageStructure of the new chiral rigid bisetherketone macrocycle produced.