The reaction of 1:2 molar ratio of anhydrous YbCl3 with sodium indenyl in tetrahydrofuran (THF) resulted in the formation of [Na(THF) 6][(η5-C9H7)3Yb(μ- Cl)Yb(η5-C9H7)3] with a good yield. X-Ray analysis demonstrates that the complex consists of a disconnected ion pair formed by [(η5-C9H7) 3Yb(μ-Cl)Yb(η5-C9H7) 3] anion and the sodium cation surrounded by six THF molecules. The complex crystallizes in the triclinic system, with space group P1 with unit-cell constants a = 1.0682(2) nm, b = 1.2687(3) nm, c = 1.2869(2) nm, α = 87.323 (1)°, β = 81.755°, γ = 88.217°, V = 1.7273(1) nm3, for Z = 1. The structure was solved by direct methods and full-matrix least-squares refinement to the final R = 0.062, Rw = 0.072. [Na(THF)6][(η5-C9H7) 3Yb(μu-Cl)Yb(η5-C9H7) 3] reacted with sodium to form (C9H7) 2Yb·2THF, the structure of which was also determined by X-ray.
In order to stabilize the organolanthanide chlorides or dichlorides, some substituted cyclopentadienes are used as ligands. At present, several kinds of substituted cyclopentadienes, e. g. CH_3C_5H_5, C_5(CH_3)_5H, (CH_3)_3SiC_5H_5, t-C_4H_9C_5H_5, CH_3CH_2CH_2- C_5H_5, etc., have been used as the ligands. Benzylcyclopentadiene was synthesized in 1936. So far, however, very few studies on benzylcyclopentadiene as a ligand used in organometallic chemistry have been found. Only benzylcyclopentadienyl iron and uranium complexes have been reported. Recently, we synthesized benzylcyclopentadienyl lanthanide dichlorides. In this note, we report the syntheses and crystal structures of bisbenzylcyclopentadienyl lanthanide chlorides.
In recent years,the organometallic ehemistry of the lanthanide metals in low oxidation states has beenactively investigated.The synthesis of the low一valent lanthanide eomPlexes has the signifieant meanings ontheory and praeti
稀土金属有机配合物合成中利用取代环戊二烯的目的在于防止轻稀土歧化.目前,已开发出的取代环戊二烯有CH 3 C 5 H 5 、C 5 (CH 3 ) 5 H、(CH 3 ) 3 SiC 5 H 5 、t-C 4 H 9 C 5 H 5 及(CH 3 OCH 2 CH 2 C 5 H 5 等多种配体.苄基环戊二烯虽早在1936年就已合成,但用它作为配体在金属有机化学中的研究极少,仅报道过它的铁、铀配合物.我们首次利用这个配体合成了其稀土二氯化物.本文报道双(苄基环戊二烯基)稀土氯化物的合成与结构.
In this paper, copper(Ⅱ)·tetra-4-(2-methoxyethanoxy-carbonyl) phthalocyanine (A) and copper(Ⅱ)-tetra 4-(2-butoxyethanoxy carbonyl) phthalocyanine (B) were synthesized and characterized by elemental analysis, FT-IR, 1H NMR and ESR. UV-vis spectra indicate that most of them are dimeric compounds in CHCl3 solution. X-ray diffraction patterns of the powder samples showed that the stacking arrangments of the molecules are inter-parallel in the tilted way. Presence of organic substituents in phthalocyanine ring somewhat lowers its thermostability. Surface(π)-area(A) isotherms for both compounds in CHCl3 solution onto subphase(water) at 20℃ showed the existence of the obvious interchange among the "gas", "liquid","solid" phases and both compounds could form a better monomolecular layer film.
> Although the synthesis of bridged-bicyclopentadienyl lanthanide complexes has been reported, the ethylene-bridged cyclopentadienyl lanthanoid complexes are not yet synthesized. We report here the synthesis and characterization of (CH 3 ) 4 C 2 (C 5 H 4 ) 2 LnCl 2 .
桥联双环戊二烯基稀土化合物的合成已有不少报道。但双碳桥联双环戊二烯基稀土化合物至今未见任何报道。我们以(CH 3 ) 4 C 2 (C 5 H 4 MgCl) 2 ·4THF(Ⅰ)与无水三氯化稀土反应,通过控制两者的比例合成了两类双碳桥联二环戊二烯基稀土氯化物,(CH 3 ) 4 C 2 (C 5 H 4 ) 2 LnCl 2 ·Mg 2 Cl 3 ·nTHF(Ⅱ)和(CH 3 ) 4 C 2 (C 5 H 4 LnCl 2 ·MgCl 2 ) 2 ·nTHF(Ⅲ),并对这两类化合物进行了表征,证实了这两类化合物的存在。