Abstract

Tetraphenylphosphorus, tetraphenylantimony, and tetraphenylbismuth mesitylene sulfonates Ph₄EOSO₂C₆H₂Me₃-2,4,6 (E = P (I), Sb (II), Bi (III)) have been synthesized in up to 91% yields by the reaction of equimolar amounts of pentaphenyl phosphorus, antimony, and bismuth compounds with mesitylene sulfonic acid in benzene. The crystal structures of these products have been determined by X-ray crystallography. Compounds I−III have also been synthesized from mesitylene sulfonic acid and tetraphenylphosphorus, tetraphenylantimony, and tetraphenylbismuth chlorides in water in up to 93% yields. Crystal I is composed of tetraphenylphosphonium cations (P−C, 1.7911(15)–1.7975(16) Å; CPC, 107.81(7)°–111.85(7)°) and mesitylene sulphonate anions (S−O, 1.4227(16)–1.4544(13) Å; OSO, 110.93(12)°–115.40(15)°). Compounds II and III are isostructural. The antimony and bismuth atoms in II and III have a distorted trigonal-bipyramidal coordination with the mesitylene sulfonate ligand in the axial position. The E−C_eq bond lengths are 2.111(3)−2.124(3) Å (II) and 2.205(3)−2.213(3) Å (III); the E−C_ax bond lengths are 2.144(3) and 2.237(3) Å, respectively; the СEO axial angles are 174.13(8)° and 173.47(9)°. The E−O distances (2.469(2) and 2.658(2) Å) exceed the sum of the covalent radii of the constituent atoms.

中文翻译：

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四苯基磷、四苯基锑和四苯基铋均三甲基磺酸盐 Ph4EOSO2C6H2Me3-2,4,6 (E = P, Sb, Bi) 的合成和结构

摘要

四苯基磷、四苯基锑和四苯基均三甲基磺酸铋 Ph ₄ EOSO ₂ C ₆ H ₂ Me ₃ -2,4,6 (E = P ( I ), Sb ( II ), Bi ( III )) 的合成率高达 91%由等摩尔量的五苯基磷、锑和铋化合物与均三甲苯磺酸在苯中反应得到。这些产品的晶体结构已通过 X 射线晶体学确定。化合物I - III还可以从均三甲苯磺酸和四苯基磷、四苯基锑和四苯基氯化铋在水中合成，产率高达 93%。晶体I由四苯基膦阳离子 (P−C, 1.7911(15)–1.7975(16) Å; CPC, 107.81(7)°–111.85(7)°) 和均三甲苯磺酸盐阴离子 (S−O, 1.4227(16) –1.4544(13) Å；OSO，110.93(12)°–115.40(15)°)。化合物II和III是同构的。II和III中的锑和铋原子与轴向位置的均三甲苯磺酸盐配体具有扭曲的三角双锥配位。E−C _eq键长为 2.111(3)−2.124(3) Å (II ) 和 2.205(3)−2.213(3) Å (三）；E−C_轴键长分别为 2.144(3) 和 2.237(3) Å；СEO轴角分别为174.13(8)°和173.47(9)°。E−O 距离（2.469(2) 和 2.658(2) Å）超过组成原子的共价半径之和。