摘要: 利用二烃基氧化锡和α-萘氧乙酸按1∶1反应,合成了8种新的有机锡化合物,{[(n-C4H9)2Sn(OOCCH2OC10H7)]2O}2(R= nBu 1,2-ClC6H4CH2 2,3-ClC6H4CH2 3,4-ClC6H4CH2 4,2-FC6H4CH2 5,3-FC6H4CH2 6, 4-FC6H4CH2 7, 4-NCC6H4CH2 8)。用元素分析、IR、 1H NMR对其结构进行了表征,并测定了化合物{[(n-C4H9)2Sn(OOCCH2OC10H7)]2O}2 (1)的晶体结构。该化合物晶体属三斜晶系,空间群P1,a=11.974(7) nm,b=1.360 5(9) nm,c=1.386 5(9) nm,α=103.940(9)°,β=104.876(8)°,γ=99.807(9)°,Z=1,V=2.053(2) nm3,Dc=1.431 Mg·m-3,μ=1.261 mm-1,F(000)=900,S=1.004,R1=0.061 0,wR2=0.151 9。结果表明,化合物1是以Sn2O2为中心的中心对称二聚体结构,内环锡和外环锡原子均为五配位的畸变三角双锥构型。 |
Abstract: The eight new organotin compounds, {[(n-C4H9)2Sn(OOCCH2OC10H7)]2O}2 (R= nBu 1,2-ClC6H4CH2 2,3-ClC6H4CH2 3,4-ClC6H4CH2 4,2-FC6H4CH2 5,3-FC6H4CH2 6, 4-FC6H4CH2 7, 4-NCC6H4CH2 8), were synthesized by the reaction of dialkyltin oxide with α-naphthyloxyacetic acid in 1∶1 molar ratio. All compounds are characterized by elemental analysis, IR, 1H and 119Sn NMR spectra, and compound {[(n-C4H9)2Sn(OOCCH2OC10H7)]2O}2(1) has been determined by X-ray single crystal diffraction. The crystal belongs to triclinic with space group P1, a=11.974(7) nm, b=1.360 5(9) nm, c=1.386 5(9) nm, α=103.940(9)°, β=104.876(8)°, γ=99.807(9)°, Z=1, V=2.053(2) nm3, Dc=1.431 Mg·m-3, μ=1.261 mm-1, F(000)=900, S=1.004, R1=0.061 0, wR2=0.151 9. The compound 1 belongs to centrosymmetric dimer structure mode with a four-membered central endo-cyclic Sn2O2 unit in which the bridged oxygen atoms are tri-coordinated. Each bridged oxygen atom also connects with an exo-cyclic tin atom. Both endo-cyclic and exo-cyclic tin atoms are five-coordinated and have coordination geometry of distorted trigonal bipyramid. CCDC: 298808. |