Bis(2,3,4,5-tetrafluorobenzoyloxy)triphenylantimony Ph₃Sb[OC(O)C₆HF₄-2,3,4,5]₂ (3) has been synthesized in 91% yield by the reaction of triphenylantimony (1) with 2,3,4,5-tetrafluorobenzoic acid (2) and tert-butyl hydroperoxide (in the mole ratio of 1:2:1) in diethyl ether. Tetraphenylantimony 2,3,4,5-tetrafluorobenzoate Ph₄SbOC(O)C₆HF₄-2,3,4,5 (5) has been obtained by the interaction between pentaphenylantimony (4) and compound 3 in benzene (95% yield), as well as by the reaction of pentaphenylantimony 4 with 2,3,4,5-tetrafluorobenzoic acid 2 (86% yield). According to the X-ray diffraction data, in compounds 3, 5 the antimony atoms have a trigonal bipyramidal coordination with the oxygen (3) or carbon and oxygen (5) atoms in axial positions. The sum of the equatorial CSbC angles in 3 and 5 is equal to 359.98(11)° and 356.52(6)°, respectively. The average value of the equatorial Sb–C bonds in 3 (2.104(3) Å) is less than in 5 (2.1132(16) Å). The Sb―O bond lengths in 3 (2.117 (2), 2.134 (2) Å) are significantly shorter than in 5 (2.2998 (13) Å). Molecular packing in crystals 3 and 5 is characterized by the presence of intermolecular contacts Sb···O = C: 3.110(3), 2.982(2) Å, and 3.233(2) Å, respectively.

双（2,3,4,5-四氟苯甲酰氧基）三苯基锑Ph ₃ Sb [OC（O）C ₆ HF ₄ -2,3,4,5] ₂（3）已通过三苯基锑反应以91％的产率合成（1）用在乙醚中的2,3,4,5-四氟苯甲酸（2）和叔丁基氢过氧化物（摩尔比为1：2：1）。通过五苯基锑（4）与化合物3的相互作用获得了2,3,4,5-四氟苯甲酸四苯基锑Ph ₄ SbOC（O）C ₆ HF ₄ -2,3,4,5（5）在苯中的收率（95％），以及五苯基锑4与2,3,4,5-四氟苯甲酸2的反应（收率86％）。根据X射线衍射数据，在化合物3，5个的锑原子具有与氧（一个三角双锥协调3）或碳和氧（5）原子的轴向位置。赤道CSbC角在3和5中的总和分别等于359.98（11）°和356.52（6）°。3（2.104（3）Å）中赤道Sb-C键的平均值小于5（2.1132（16）Å）。Sb-O键长度为3（2.117（2），2.134（2）Å）明显短于5（2.2998（13）Å）。晶体3和5中的分子堆积的特征是存在分子间接触Sb···O = C：分别为3.110（3），2.982（2）Å和3.233（2）Å。