对硝基苯甲酸二丁基锡酸酯的合成与晶体结构

Synthesis and Crystal Structure of Dibutyltin Esters of P-Nitrobenzoic Acid

摘要: 我们利用二丁基氧化锡、对硝基苯甲酸在摩尔比1:2下进行反应合成了化合物Bu₂Sn[OOCC₆H₄(NO₂-p)]₂。通过元素分析、红外光谱、核磁共振氢谱以及X-射线单晶衍射测定了化合物的结构。该化合物晶体属单斜晶系，空间群Cc，a = 1.5604(5) nm，b = 0.7007(2) nm，c = 2.2816(7) nm；α = 90˚，β = 103.599(5)˚，γ = 90˚；Z = 4，V = 2.4247(13) nm³，Dc = 1.548 mg/m³，μ(MoKα) = 1.102 mm⁻¹，F(000) = 1144，R = 0.0373，wR = 0.0964。该化合物中与锡原子键连的四个氧原子占据了四角双锥的赤道平面，两个丁基碳原子占据轴向位置。其几何形状是变形的四角双锥结构。

Abstract: The title organotin (IV) compound Bu₂Sn[OOCC₆H₄(NO₂-p)]₂ has been synthesized by the reaction of dibutyltin oxide with p-nitrobenzoic acid in 1:2 molar ratio. The compound was characterized by elemental analysis, FT-IR, 1HNMR spectra and X-ray crystallography. The crystal belongs to triclinic space group Cc, a = 1.5604(5) nm, b = 0.7007(2) nm, c = 2.2816(7) nm; α = 90˚, β = 103.599(5)˚, γ = 90˚; Z = 4, V = 2.4247(13) nm³, Dc = 1.548 mg/m³, μ(MoKα) = 1.102 mm⁻¹, F(000) = 1144, R = 0.0373, wR = 0.0964. In the compound Sn atom exhibited six-coordinate with four oxide atoms on the orbital panel and two butyls in symmetry distribution against the plain, which result in compressed tetrahedron bipyramidal geometry.