济宁学院学报
濟寧學院學報
제저학원학보
JOURNAL OF JINING UNIVERSITY
2013年
6期
32-35
,共4页
高中军%公维强%刘晓东%王晓梅%蒋浩
高中軍%公維彊%劉曉東%王曉梅%蔣浩
고중군%공유강%류효동%왕효매%장호
5-溴吡啶甲酸%合成%晶体结构
5-溴吡啶甲痠%閤成%晶體結構
5-추필정갑산%합성%정체결구
5-Br-omonicotinic acid%synthesis%X-ray crystal structure
5-溴吡啶甲酸与二丁基氧化锡反应,制得新配合物[n-Bu2Sn(OCOC5H3N-3-Br-5)2]n.通过元素分析、红外光谱对其结构进行了表征,用X-射线单晶衍射测定了配合物的晶体结构.该配合物晶体属于三斜晶系,空间群为Pī,晶胞参数a=8.068(2)?,b=10.044(3)?,c=15.158(4)?,α=76.001(4)o,β=80.659(4)o,γ=79.932(4)o,V=1164.2(6)?3,Z=2,μ=4.557mm-1,Dc=1.811Mg?m-3,F(000)=620,R=0.0350,wR=0.0831,GOF=1.001.测试结果表明,该化合物中每个5-溴吡啶甲酸分子通过两个羧基氧原子与锡原子配位,其中一个吡啶环氮原子与相邻锡原子配位使整个化合物呈一维链状结构,而另一吡啶环氮原子与周围锡原子不配位.
5-溴吡啶甲痠與二丁基氧化錫反應,製得新配閤物[n-Bu2Sn(OCOC5H3N-3-Br-5)2]n.通過元素分析、紅外光譜對其結構進行瞭錶徵,用X-射線單晶衍射測定瞭配閤物的晶體結構.該配閤物晶體屬于三斜晶繫,空間群為Pī,晶胞參數a=8.068(2)?,b=10.044(3)?,c=15.158(4)?,α=76.001(4)o,β=80.659(4)o,γ=79.932(4)o,V=1164.2(6)?3,Z=2,μ=4.557mm-1,Dc=1.811Mg?m-3,F(000)=620,R=0.0350,wR=0.0831,GOF=1.001.測試結果錶明,該化閤物中每箇5-溴吡啶甲痠分子通過兩箇羧基氧原子與錫原子配位,其中一箇吡啶環氮原子與相鄰錫原子配位使整箇化閤物呈一維鏈狀結構,而另一吡啶環氮原子與週圍錫原子不配位.
5-추필정갑산여이정기양화석반응,제득신배합물[n-Bu2Sn(OCOC5H3N-3-Br-5)2]n.통과원소분석、홍외광보대기결구진행료표정,용X-사선단정연사측정료배합물적정체결구.해배합물정체속우삼사정계,공간군위Pī,정포삼수a=8.068(2)?,b=10.044(3)?,c=15.158(4)?,α=76.001(4)o,β=80.659(4)o,γ=79.932(4)o,V=1164.2(6)?3,Z=2,μ=4.557mm-1,Dc=1.811Mg?m-3,F(000)=620,R=0.0350,wR=0.0831,GOF=1.001.측시결과표명,해화합물중매개5-추필정갑산분자통과량개최기양원자여석원자배위,기중일개필정배담원자여상린석원자배위사정개화합물정일유련상결구,이령일필정배담원자여주위석원자불배위.
A organotin compound [n-Bu2Sn (OCOC5H3N-3-Br-5)2]n has been synthesized by the reaction of (n-Bu)2SnO with 5-Br-omonicotinic acid in 1:2 molar ratio and characterized by elemental analysis, IR, spectroscopy. The crystal structure has been determined by X-ray single crystal diffraction. The crystal belongs to Triclinic space group Pī, with a=8.068(2) ?, b=10.044(3) ?, c=15.158(4) ?,α=76.001(4)o,β=80.659(4)o,γ=79.932(4)o ,V=1164.2 (6) ? 3, Z=2, μ=4.557 mm-1, Dc=1.811 Mg?m-3, F(000)=620, R=0.0350, wR=0.0831, GOF=1.001. In the compound, each carboxylate moiety of 5-Br-omonicotinic acid is involved in coordination to one Sn atom via two O-atoms, and the N-atom of one pyridine-ring coordinates to the neighboring Sn atom which leads to a polymeric chain. And the N-atom of the other pyridine-ring is dissociative.