二(2-吡啶甲酸)二(邻氟苄基)锡和一维链状4-吡啶甲酸三(邻氟苄基)锡的合成和晶体结构
Synthesis and Crystal Structure of the Di(o-fluorobenzyl)tin Bis(2-picolinate) and the Tri(o-fluorobenzyl)tin 4-Picolinate
作者单位
张复兴 衡阳师范学院化学与材料科学系衡阳 421008 
邝代治 衡阳师范学院化学与材料科学系衡阳 421008 
王剑秋 衡阳师范学院化学与材料科学系衡阳 421008 
冯泳兰 衡阳师范学院化学与材料科学系衡阳 421008 
陈志敏 衡阳师范学院化学与材料科学系衡阳 421008 
摘要: μ-氧-双[三(邻氟苄基)锡]与2-吡啶甲酸或4-吡啶甲酸在苯溶剂中反应合成有机锡配合物二(2-吡啶甲酸)二(邻氟苄基)锡(1)和一维链状4-吡啶甲酸三(邻氟苄基)锡(2),经X射线衍射方法测定了新化合物的晶体结构。配合物(1)属四方晶系,空间 群为I41/a,晶体学参数:a=1.562 0(3) nm,b=1.562 0(3) nm,c=1.984 7(4) nm,α=β=γ=90°,V=4.842 4(16) nm3,Z=8,Dc=1.594 Mg·m-3, μ(Mo Kα)=11.06 cm-1,F(000)=2 320,R1=0.024 3,wR=0.062 5。配合物(2)属单斜晶系,空间群为P21/n,晶体学参数:a=0.869 8(3) nm,b=1.880 5(7) nm,c=1.475 1(5) nm,β=90.937(6)°,V=2.412 3(15) nm3,Z=4,Dc=1.564 Mg·m-3,μ(Mo Kα)=11.07 cm-1,F(000)=1 136,R1=0.028 8,wR2=0.057 9;配合物1为单体结构,中心锡为六配位畸变八面体构型。配合物2通过4-吡啶甲酸配体氮原子的桥联,形成五配位三角双锥型的链状结构。
关键词: 有机锡配合物  2-吡啶甲酸  4-吡啶甲酸  合成  晶体结构
基金项目: 
Abstract: The Di(o-fluorobenzyl)tin Bis(2-picolinate) (1) and the one-dimensional chain tri(o-fluorobenzyl)tin 4-picolinate (2) have been synthesized. The crystal structures of the complexes were determined by X-ray diffraction.The crystal 1 belongs to Tetragonal space group I41/a with a=1.562 0(3) nm, b=1.562 0(3) nm, c=1.984 7(4) nm, α=β=γ=90°, V=4.842 4(16) nm3, Z=8, Dc=1.594 Mg·m-3, μ(Mo Kα)=11.06 cm-1, F(000)=2 320, R1=0.024 3, wR=0.062 5. The crystal 2 belongs to Monoclinic space group P21/n with a=0.869 8(3) nm, b=1.880 5(7) nm, c=1.475 1(5) nm, β=90.937(6)°, V=2.412 3(15) nm3, Z=4, Dc=1.564 Mg·m-3, μ(Mo Kα)=11.07 cm-1, F(000)=1 136, R1=0.028 8, wR2=0.057 9. The crystal 1 is monomeric,with six-coordinated tin atom in a distorted octahedron geometry. In the crystal 2, the tin atom rendered five-coordinate in trigonal bipyramid structure by bridging pyridine N atom,resulting the one-dimensional chain polymer. CCDC: 283823, 1; 283822, 2.
Keywords: organotin  2-picolinic acid  4-picolinic acid  synthesis  crystal structure
 
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张复兴,邝代治,王剑秋,冯泳兰,陈志敏.二(2-吡啶甲酸)二(邻氟苄基)锡和一维链状4-吡啶甲酸三(邻氟苄基)锡的合成和晶体结构[J].无机化学学报,2006,22(1):7-12.
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