无机化学学报
無機化學學報
무궤화학학보
JOURNAL OF INORGANIC CHEMISTRY
2012年
2期
386-390
,共5页
有机锡配合物%氧化-4-吡啶甲酸%合成%晶体结构
有機錫配閤物%氧化-4-吡啶甲痠%閤成%晶體結構
유궤석배합물%양화-4-필정갑산%합성%정체결구
organotin compound%pyridine-4-carboxylic acid N-oxide%synthesis%crystal structure
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=0.0529,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.
利用雙三丁基氧化錫與氧化4吡啶甲痠(HOCOC5H4NO)以物質的量比1∶2反應,閤成瞭有機錫配閤物[Bu3Sn(OCOC5H4NO)]n.通過元素分析、紅外光譜和覈磁共振氫譜對其結構進行瞭錶徵,用X射線單晶衍射測定瞭它的晶體結構.結果錶明,該配閤物晶體屬單斜晶繫,空間群為C2/c,晶胞參數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=0.0529,wR=0.192 1,GOF=1.013.在配閤物中錫原子由氧化-4-吡啶甲痠橋聯為五配位的畸變的三角雙錐構型.氧化-4-吡啶甲痠配體中N-O基糰中的氧原子和另一配體中的羧基氧原子與中心錫原子配位,形成無限一維鏈狀有機錫配閤物.該配閤物具有良好的熱穩定性和較高的抗腫瘤活性.
이용쌍삼정기양화석여양화4필정갑산(HOCOC5H4NO)이물질적량비1∶2반응,합성료유궤석배합물[Bu3Sn(OCOC5H4NO)]n.통과원소분석、홍외광보화핵자공진경보대기결구진행료표정,용X사선단정연사측정료타적정체결구.결과표명,해배합물정체속단사정계,공간군위C2/c,정포삼수a=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=0.0529,wR=0.192 1,GOF=1.013.재배합물중석원자유양화-4-필정갑산교련위오배위적기변적삼각쌍추구형.양화-4-필정갑산배체중N-O기단중적양원자화령일배체중적최기양원자여중심석원자배위,형성무한일유련상유궤석배합물.해배합물구유량호적열은정성화교고적항종류활성.
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.