CAJ | 학술논문

三氯化稀土依次与等摩尔的甲基环戊二烯基钠和环戊二烯基钠在四氢呋喃(THF)中反应,合成了4个新的混配型茂基稀土氯化物Ln(C5H5)(C5H4CH3)Cl[Ln=Y(1), Gd(2), Er(3), Yb(4)]. 在THF中加热回流,环戊二烯能质解化合物4的甲基环戊二烯基配体, 得到同环配合物Yb(C5H5)2Cl(5). 所有这些化合物都经过了元素分析、红外和质谱表征,其中配合物2和5的结构还得到单晶X射线分析确证.
삼록화희토의차여등마이적갑기배무이희기납화배무이희기납재사경부남(THF)중반응,합성료4개신적혼배형무기희토록화물Ln(C5H5)(C5H4CH3)Cl[Ln=Y(1), Gd(2), Er(3), Yb(4)]. 재THF중가열회류,배무이희능질해화합물4적갑기배무이희기배체, 득도동배배합물Yb(C5H5)2Cl(5). 소유저사화합물도경과료원소분석、홍외화질보표정,기중배합물2화5적결구환득도단정X사선분석학증.
The reaction of LnCl3 and NaC5H4CH3, followed by reaction with an equivalent of NaC5H5,forms mixed-ring dicyclcopentadienyl lanthanide chlorides CpCp'LnCl (Cp=C5H5, Cp'=C5H4CH3) [Ln=Y(1), Gd(2), Er(3), Yb(4)]. Treatment of complex 4 with an excess of cyclopentadiene results in the abstract of the C5H4CH3-ligand to generate the corresponding homogenous-ring complex Cp2YbCl(THF)(5). All the complexes were characterized by elemental analysis, IR and MS spectroscopies. The crystal structures of 2 and 5 were determined by single crystal X-ray diffraction methods. Crystals of 2 are orthorhombic, space group P212121, with unit cell dimensions a=8.925(5), b=19.562(8), c=7.109(4) (A), V=1241(1) (A)3 and Dc=1.803 g*cm-3 for Z=4. Complex 2 has a chain structure with bridging chlorine atoms. The average Gd-C and Gd-Cl distances are 2.66(3) and 2.71(1) (A), respectively. 5 crystallizes in orthorhombic system, space group Pnma with a=13.140(4), b=1.820(3), c=9.341(2) (A), V=1446.4 (A)3 and Dc=1.886 g*cm-3. In 5 two Cp ring centroids, one chlorine atom and one oxygen atom of THF describe a distorted tetrahedron around the central ion of ytterbium. The average distance of Yb-C (ring) is 2.57(1) (A). The average Yb-Cl and Yb-O (THF) distances are 2.502(4) and 2.270(8) (A), respectively.