环戊二烯-12-钼硅杂多四丁基铵电荷转移盐的合成、表征与晶体结构

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以环戊二烯与 1 2 钼硅杂多四丁基铵为原料 ,采用光化学法合成了一种新型电荷转移盐 (Bu4N) 4(C5 H6 ) [HSiMoVI11MoVO40 ]。用元素分析、IR、CV、固体漫反射电子光谱、ESR进行了表征。X 射线晶体结构测定其晶体属三斜晶系 ,空间群P1 ,晶胞参数a =1 4.347(3) ,b =1 4.42 3(3) ,c =2 7.1 5 8(5 ) ,α =96 .90 (3) ,β =1 0 4.1 8(3) ,γ =98.2 0 (3)° ,V =5 32 2 (2 ) 3,Z =2 ,Mr=2 85 5 .30 ,Dc=1 .782 g·cm-3,F(0 0 0 ) =2 86 0 ,R =0 .0 71 9,wR =0 .1 983。标题化合物由 1个环戊二烯、4个Bu4N+阳离子和 1个 [SiMoVI11MoVO40 ]4 -阴离子构成。 A novel charge-transfer salt (Bu4N) 4 (C5H6) [HSiMoVI11MoVO40] was synthesized by the photochemical method using cyclopentadienyl and 1, 2 molybdenum-silicon heterobutene tetrabutylammonium as raw material. It was characterized by elemental analysis, IR, CV, solid-state diffuse reflectance spectroscopy and ESR. X-ray crystal structure of the crystal is determined triclinic, space group P1, cell parameters a = 1 4.347 (3), b = 1 4.42 3 (3), c = 2 7.15 8 (5), α = 96 .90 (3), β = 1 0 4.1 8 (3), γ = 98.2 0 (3) °, V = 5 32 2 (2) 3, Z = 2, Mr = 2 85 5 .30, Dc = 1 .782 g · cm -3, F (0 0 0) = 2 86 0, R = 0 .0 71 9, wR = 0 .1 983. The title compound consists of 1 cyclopentadiene, 4 Bu4N + cations and 1 [SiMoVI11MoVO40] 4 - anion.
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