二硫二茂铁的合成及其晶体结构

Synthesis and Crystal Structure of Diferrocenyl Disulfide

用AlI3作还原剂 ,还原二茂铁磺酰氯得到二硫二茂铁 .通过元素分析 ,IR ,1HNMR和13CNMR对化合物进行了表征 .用X射线单晶衍射法测定了该化合物的晶体结构 .结果表明 ,晶体属单斜晶系 ,P2 1空间群 ,a =0 61881(4)nm ,b =1 0 32 31(9)nm ,c =1 390 5 6(11)nm ,β =94 179(3)° ,V =0 85 5 93(12 )nm3,Dc=1.62 8g/cm3,μ =1 870mm-1,F(0 0 0 ) =444 ,Z =2 ,R1=0 0 2 7,wR2 =0 0 678.

Diferrocenyl disulfide was synthesized by the reduction of ferrocenesulfonyl chloride using aluminum iodide as a reducing reagent. The structure was characterized by elemental analysis, IR, H-1 NMR and C-13 NMR spectra. Crystal structure was determined by X-ray diffraction analysis. The crystal data belong to monoclinic space group with unit cell dimensions a = 0.61881(4) nm, b = 1.03231(9) nm, c = 1.39056 (11) nm, beta = 94.179(3)degrees, V = 0.85593(12) nm(3), D-c =1.628 g/cm(3), mu =1.870 mm(-1), F(000) -444, Z =2, R-1 =0.027 and wR(2) =0.0678.