Design, Hydrothermal Synthesis, Crystal Structure, and Antioxidant Properties of Non‐Centrosymmetric SbF ₃

ABSTRACT The crystallization of highly hygroscopic antimony trifluoride by a hydrothermal synthetic technique has been reported for the first time. A detailed structural investigation, along with antioxidant properties, has been performed using synthesized crystalline materials. The full set of single‐crystal X‐ray diffraction data was collected under N 2 atmosphere, and strict precautions were taken to prevent hydrolysis. The study revealed that SbF 3 crystallizes in an orthorhombic system with a non‐centrosymmetric space group C 2 cm and unit cell parameters a = 4.90(4) Å, b = 7.38(6) Å, c = 7.20(6) Å, with α = β = γ = 90°, and Z = 4. Comparative studies based on Sb‐F distances revealed that it is in close agreement with those previously reported Sb–F distances in Sb 3 O 4 F, L‐SbOF, α‐Sb 3 O 2 F 5, etc. Energy‐dispersive X‐ray spectroscopy (EDX) confirmed the expected elemental composition and scanning electron microscopy (SEM) revealed the formation of plate‐shaped particles. The antioxidant property of both synthesized and commercial SbF 3 was investigated using the 1,1‐diphenyl‐2‐picrylhydrazyl (DPPH) free radical scavenging assay. The crystalline SbF 3 exhibited strong radical scavenging activity up to 91% within a 3h reaction period, demonstrating significantly antioxidant activity than commercially available SbF 3 . This investigation establishes a reproducible pathway for the synthesis of high‐quality single crystals of SbF 3 and provides the first complete crystallographic description of this compound, contributing valuable structural data to the ICSD. Furthermore, comparative studies confirm that the radical scavenging activity of SbF 3 is significantly higher than that of some other p‐block element‐based catalysts.