无机化学学报
無機化學學報
무궤화학학보
JOURNAL OF INORGANIC CHEMISTRY
2010年
6期
1083-1088
,共6页
贾斌%张万青%童红波%郝俊生%刘滇生
賈斌%張萬青%童紅波%郝俊生%劉滇生
가빈%장만청%동홍파%학준생%류전생
合成%结构%氮杂烯丙基化合物
閤成%結構%氮雜烯丙基化閤物
합성%결구%담잡희병기화합물
synthesis%structure%1-azaallyl complex
本文以[(Me2)NCH2C6H4CHSiMe2(NMe2)]Li(TMEDA)与叔丁腈为原料按1:1加成得到氮杂烯丙基的锂化合物[{(Me2)NCH2C6H4}CHC(tBu)NSiMe2(NMe2)Li(TMEDA)]即1.然后用乙醚或四氢呋喃作溶剂化合物1和二氯化亚铁或二氯化钻按2:1反应得到氮杂烯丙基铁或钴的化合物分别为2和3.通式为M[{(Me2)NCH2C6H4}CHC(tBu)NSiMe2(NMe2)2(M=Fe(2),Co(3)).化合物1,2和3的结构分别用1H NMR,13C NMR,元素分析和X-射线单晶衍射技术进行了表征.晶体结构表明化合物2和3结构类似,都是以金属为对称中心的硅桥联的端基氮配位的氮杂烯丙基化合物.
本文以[(Me2)NCH2C6H4CHSiMe2(NMe2)]Li(TMEDA)與叔丁腈為原料按1:1加成得到氮雜烯丙基的鋰化閤物[{(Me2)NCH2C6H4}CHC(tBu)NSiMe2(NMe2)Li(TMEDA)]即1.然後用乙醚或四氫呋喃作溶劑化閤物1和二氯化亞鐵或二氯化鑽按2:1反應得到氮雜烯丙基鐵或鈷的化閤物分彆為2和3.通式為M[{(Me2)NCH2C6H4}CHC(tBu)NSiMe2(NMe2)2(M=Fe(2),Co(3)).化閤物1,2和3的結構分彆用1H NMR,13C NMR,元素分析和X-射線單晶衍射技術進行瞭錶徵.晶體結構錶明化閤物2和3結構類似,都是以金屬為對稱中心的硅橋聯的耑基氮配位的氮雜烯丙基化閤物.
본문이[(Me2)NCH2C6H4CHSiMe2(NMe2)]Li(TMEDA)여숙정정위원료안1:1가성득도담잡희병기적리화합물[{(Me2)NCH2C6H4}CHC(tBu)NSiMe2(NMe2)Li(TMEDA)]즉1.연후용을미혹사경부남작용제화합물1화이록화아철혹이록화찬안2:1반응득도담잡희병기철혹고적화합물분별위2화3.통식위M[{(Me2)NCH2C6H4}CHC(tBu)NSiMe2(NMe2)2(M=Fe(2),Co(3)).화합물1,2화3적결구분별용1H NMR,13C NMR,원소분석화X-사선단정연사기술진행료표정.정체결구표명화합물2화3결구유사,도시이금속위대칭중심적규교련적단기담배위적담잡희병기화합물.
The N-silyl-Ni-(2-((dimethylamino)methyl)benzyl)-N,N,l,l-tetramethylsilanamiolithium 1-azaally compound [{(Me2)NCH2C6H4}CHC(tBu)NSiMe2(NMe2)Li(TMEDA)] (1) was synthesized by interaction of [(Me2)NCH2C6H4 CHSiMe2(NMe2)]Li(TMEDA) with one equivalent of tertbutyronitrile (tBuCN). The derivative iron(Ⅱ) and cobalt(II) compounds were produced by the treatment of 1 with FeCl2 or CoCl2 in tetrahydrofuran or diethylether at zero temperature, respectively, with the general formula M[{(Me2)NCH2C6H4}CHC(tBu)NSiMe2(NMe2)]2 (M=Fe (2), Co (3)). The 1-azaally complexes 1,2 and 3 were also characterized by X-ray single crystal diffraction and NMR analysis. Structural analyses of 2 and 3 reveal that their molecular structures are very similar. The structure of the centrosymmetric crystalline Fe(Ⅱ) or Co (Ⅱ) is unusually within the present series of homoleptic metal (Ⅱ) 1-azaallyls in that it is an k1-enamido metal complex. CCDC: 771795, 1; 771796, 2; 771797, 3.