无机化学学报
無機化學學報
무궤화학학보
JOURNAL OF INORGANIC CHEMISTRY
2012年
10期
2236-2240
,共5页
张东娣%王科%燕庆霞%马鹏涛%王敬平
張東娣%王科%燕慶霞%馬鵬濤%王敬平
장동제%왕과%연경하%마붕도%왕경평
有机硅%三缺位磷钨酸盐%晶体结构%合成
有機硅%三缺位燐鎢痠鹽%晶體結構%閤成
유궤규%삼결위린오산염%정체결구%합성
organosilyl%trivacant tungstophosphate%crystal structure%synthesis
通过三缺位Keggin结构杂多阴离子[α-A -PW9O34]9-和二氯甲基苯基硅烷在乙腈溶液中反应,合成了一例结构新颖的甲基苯基硅衍生物[(C4H9)4N]3[α-A-PW9O34(C6H5SiCH3)3] (1),并对其进行元素分析,红外光谱,紫外光谱,热分析和X-射线单晶衍射等表征.该配合物属于三方晶系,空间群为R3m,晶胞参数:a=2.261 3(2) nm,b=2.261 3(2) nm,c=1.797 6(4) nm,V=7.960 2(18) nm3,Z=3.在配合物中,阴离子[α-A -PW9O34(C6H5SiCH3)3]3]3-呈C3v对称,3个甲基苯基硅基团连接在三缺位的阴离子[α-A -PW9O34]99-表面,整个阴离子显示“开放结构”.
通過三缺位Keggin結構雜多陰離子[α-A -PW9O34]9-和二氯甲基苯基硅烷在乙腈溶液中反應,閤成瞭一例結構新穎的甲基苯基硅衍生物[(C4H9)4N]3[α-A-PW9O34(C6H5SiCH3)3] (1),併對其進行元素分析,紅外光譜,紫外光譜,熱分析和X-射線單晶衍射等錶徵.該配閤物屬于三方晶繫,空間群為R3m,晶胞參數:a=2.261 3(2) nm,b=2.261 3(2) nm,c=1.797 6(4) nm,V=7.960 2(18) nm3,Z=3.在配閤物中,陰離子[α-A -PW9O34(C6H5SiCH3)3]3]3-呈C3v對稱,3箇甲基苯基硅基糰連接在三缺位的陰離子[α-A -PW9O34]99-錶麵,整箇陰離子顯示“開放結構”.
통과삼결위Keggin결구잡다음리자[α-A -PW9O34]9-화이록갑기분기규완재을정용액중반응,합성료일례결구신영적갑기분기규연생물[(C4H9)4N]3[α-A-PW9O34(C6H5SiCH3)3] (1),병대기진행원소분석,홍외광보,자외광보,열분석화X-사선단정연사등표정.해배합물속우삼방정계,공간군위R3m,정포삼수:a=2.261 3(2) nm,b=2.261 3(2) nm,c=1.797 6(4) nm,V=7.960 2(18) nm3,Z=3.재배합물중,음리자[α-A -PW9O34(C6H5SiCH3)3]3]3-정C3v대칭,3개갑기분기규기단련접재삼결위적음리자[α-A -PW9O34]99-표면,정개음리자현시“개방결구”.
A methylphenylsilyl group-substituted derivative [(C4H9)4N]3[α-A-PW9O34(C6H5SiCH3)3] (1) has been obtained by reaction of the trivacant [α-A-PW9O34]9- anion with dichloromethylphenylsilane C6H5SiCH3Cl2 in acetonitrile.The new complex was characterized by elemental analysis,IR spectra,UV spectra,thermogravimetric analysis and X-ray crystallography.The compound 1 crystallizes in the trigonal space group R3m,with lattice constants a=2.261 3(2) nm,b=2.261 3(2) nm,c=1.797 6(4) nm,V=7.960 2(18) nm3,and Z=3.The polyoxoanion [α-A-PW9O34(C6H5SiCH3)3]3- has a structure of virtual C3v symmetry with three C6H5SiCH3 groups grafted on the surface of the trivacant tungstophosphate and displays an "open-structure".CCDC:830334.