{[(n-Bu)_2Sn(O_2CCH═CHAr)]_2O}_2的合成、表征和{[(n-Bu)_2Sn(O_2CCH═CHPh)]_2O}_2的晶体结构

Synthesis and Characterization of {[(n-Bu)_2Sn (O_2CCH═CHAr)]_2O}_2 and Crystal Structure of {[(n-Bu)_2Sn (O_2CCH═CHPh)]_2O}_2

利用 (n Bu) 2 SnO与ArCHCHCO2 H反应 ,合成 5个二聚二丁基锡芳基丙烯酸酯氧化物 {[(n Bu) 2 Sn(O2 CCHCHAr) ] 2 O}2 .通过元素分析、红外光谱和核磁共振氢谱对其结构进行了表征 .用X射线单晶衍射测定了 {[(n Bu) 2 Sn (O2 CCHCHPh) ] 2 O}2 ( 1)的晶体结构 ,结果表明 ,化合物 1是以Sn2 O2 四面体为中心的 ,中心对称的二聚体结构 ,内环锡为五配位的畸变三角双锥构型 ,外环锡为六配位的畸变加帽体三角双锥结构 .该化合物属三斜晶系 ,空间群P1- ,a =1 0 172( 11)nm ,b =1 3 80 4( 16)nm ,c =1 470 3 ( 17)nm ,α =10 6 75 0 ( 18)° ,β =10 5 61( 2 ) )° ,γ =10 0 2 95 ( 18)° ,Z =1,V =1 82 9( 4 )nm-3 ,Dc=1 413g/m3 ,μ =1 40 0mm-1 ,F( 0 0 0 ) =792 ,R =0 0 5 5 9,wR =0 12 5 0 .

The five organotin compounds {[( n Bu) 2Sn (O 2CCH[FY=,1]CHAr)] 2O} 2 were synthesized by the reaction of ( n Bu) 2SnO with ArCH 2O} 2 were synthesized by the reaction of ( n Bu) 2SnO with ArCHCHCO 2H in 1∶1 molar ratio. The crystal structure of {[( n Bu) 2Sn(O 2CCH[FY=,1]CHPh)] 2O} 2 was determined by X ray single crystal diffraction. This compound belongs to centrosymmetric dimer structure mode with a four membered central endo cyclic Sn 2O 2 unit in which the bridged oxygen atoms are tri coordinated. Each bridged oxygen atom also connects with an exo cyclic tin atom. The endo cyclic tin atoms are five coordinated and have coordination geometry of distorted trigonal bipyramid. The exo cyclic tin atoms are six coordinated and have coordination geometry of capped trigonal bipyramid with very similarly distorted mode. The crystal belongs to triclinic with space group P 1 2O} 2 was determined by X ray single crystal diffraction. This compound belongs to centrosymmetric dimer structure mode with a four membered central endo cyclic Sn 2O 2 unit in which the bridged oxygen atoms are tri coordinated. Each bridged oxygen atom also connects with an exo cyclic tin atom. The endo cyclic tin atoms are five coordinated and have coordination geometry of distorted trigonal bipyramid. The exo cyclic tin atoms are six coordinated and have coordination geometry of capped trigonal bipyramid with very similarly distorted mode. The crystal belongs to triclinic with space group P 1-, a =1 0172(11) nm, b =1 3804(16) nm, c =1 4703(17) nm, α = 106 750(18)°, β =105 61(2)°, γ =100 295(18)°, Z =1, V =1 829(4) nm -3 , D c=1 413 g/m 3, μ =1 400 mm -1 , F (000)=792, R =0 0559, wR =0 1250.