三苄基和三丁基锡4-吡啶甲酸酯聚合物的合成、性质及晶体结构

用三苄基氯化锡及三丁基氯化锡与4-吡啶甲酸钠反应,分别合成了三苄基锡4-吡啶甲酸酯(1)和三丁基锡-4-吡啶甲酸酯(2),并进行了红外光谱、核磁共振氢谱及质谱表征.X射线单晶衍射分析结果表明,化合物1属单斜晶系,P2₁/n空间群,晶胞参数:a=0.96564(8)nm,b=1.64085(14)nm,c=1.49403(13)nm,β=97.681(2)₀,V=2.3460(3)nm₃,Z=4,D_c=1.456g/cm³.化合物2属单斜晶系,P2₁/n空间群,晶胞参数:a=0.96673(14)nm,b=2.3845(4)nm,c=0.97071(14)nm,β=112.463(3)o,V=2.0679(5)nm₃,Z=4,D_c=1.324g/cm³.两个化合物均通过4-吡啶甲酸配体的氮原子桥联,形成五配位三角双锥构型的一维无限链聚合物.

Synthesis and Crystal Structure of the Polymeric Tribenzyltin 4-Picolinate and Tributyltin 4-Picolinate

Tribenzyltin 4-picolinate(1) and tributyltin 4-picolinate(2) were synthesized by the reaction of sodium 4 picolinate with the tribenzyltin chlorideor tributyltin chloride and were characterized by IR, ¹H NMRand MS. Their crystal structures were determined by X-ray single crystal diffraction. The crystal 1 crystallizes in monoclinic, space group P2₁/n with a=0.96564(8) nm, b=1.64085(14) nm, c= 1.49403(13) nm, β =97.681(2)^o, V=2.3460(3) nm³, Z=4, D_c=1.456 g/cm³, and crystal 2 in monoclinic, space group P₂ 1/c with a=0.96673(14) nm, b=2.3845(4) nm, c=0.97071(14) nm, β =112.463(3)^o, V=2.0679(5) nm³, Z=4, D_c=1.324 g/cm³. In crystals 1 and 2, the tin atom rendered five coordinate in trigonal bipyramidal structure by bridging pyridine Natom and the resulted structures are one dimensional infinite chain polymer.