氧化-4-吡啶甲酸桥联的一维链状三丁基锡配合物的合成与晶体结构

利用双三丁基氧化锡与氧化-4-吡啶甲酸(HOCOC5H4NO)以物质的量比1∶2反应,合成了有机锡配合物Bu3Sn(OCOC5H4NO)]n。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它的晶体结构。结果表明,该配合物晶体属单斜晶系,空间群为C2/c,晶胞参数a=2.002 8(9)nm,b=1.224 7(6)nm,c=1.913 6(12)nm,β=119.145(6)°,Z=8,V=4.166(4)nm3,Dc=1.365 g.cm-3,μ=1.239 mm-1,F(000)=1 760,R=0.052 9,wR=0.192 1,GOF=1.013。在配合物中锡原子由氧化-4-吡啶甲酸桥联为五配位的畸变的三角双锥构型。氧化-4-吡啶甲酸配体中N-O基团中的氧原子和另一配体中的羧基氧原子与中心锡原子配位,形成无限一维链状有机锡配合物。该配合物具有良好的热稳定性和较高的抗肿瘤活性。

Synthesis and Crystal Structure of the One-Dimensional Chain Tributyltin Compound Bridged by Pyridine-4-carboxylic Acid N-Oxide

An organotin compound Bu3Sn(OCOC5H4NO)]n has been synthesized by the reaction of bistributyltin oxide with pyridine-4-carboxylic acid N-oxide(HOCOC5H4NO) in molar ratio of 1∶2 and characterized by elemental analysis,IR and 1H NMR.The crystal structure has been determined by X-ray single crystal diffraction.The crystal belongs to monoclinic space group C2/c,with a=2.002 8(9) nm,b=1.224 7(6) nm,c=1.913 6(12) nm,β=119.145(6)°,Z=8,V=4.166(4) nm3,Dc=1.365 g·cm-3,μ=1.239 mm-1,F(000)=1 760,R=0.052 9,wR=0.192 1,GOF =1.013.In the compound,tin atoms are five-coordinated distorted trigonal bipyramid configuration with bridging pyridine-4-carboxylic acid N-oxide.A one-dimensional linear polymer is formed through an interaction between the central tin atom and two O atoms.One O atom is from N-O and the other is from carboxyl group of another ligand.The compound exhibits good thermal stability and high antitumor activity.CCDC: 821908.