Zhongsheng Jin

Synthesis and characterization of binuclear organolanthanide complexes involving cyclopentadienyl and n-propyloxide ligands. X-ray crystal structure of [(C5H5)2Yb(μ-OCH2CH2CH3)]2

By the reaction of Cp3Ln (Cp = C5H5; Ln = Dy, Ho, Yb) with equimolar n-propyl alcohol in THF (tetrahydrofuran) at room temperature three new binuclear organolanthanide complexes, [CP2Ln(mu-OCH2CH2CH3)]2 (Ln = Dy, Ho, Yb), have been synthesized, as shown by X-ray single-crystal structure analysis for the complex [Cp2Yb(mu-OCH2CH2CH3)]2. All the complexes were characterized by elemental analysis, IR and MS spectra. The Yb2O2 unit is planar, and the ytterbium atom is coordinated by two Cp ring centroids and two oxygen atoms of two n-propyloxide ligands to form a distorted tetrahedral geometry. The average Yb-C (Cp) bond distance is 2.589(17) angstrom. The average Yb-O distance is 2.199(5) angstrom. The Yb-Yb separation [3.521(1) angstrom] indicates that no metal-metal interaction is present.

Synthesis and crystal structure of [Me4C2Cp2SmCl.THF]2

Abstract Me4C2(C5H4MgCl)2(THF) (THF = tetrahedrofuran) reacts with anhydrous SmCl3 in THF to give [Me4C2Cp2SmCl · THF]2. The molecule is a dimer. Sm1 and Sm2 are bridged unsymmetrically by two chlorine atoms [Sm(1)Cl(1) 2.787(2), Sm(1)Cl(2) 2.848(2), Sm(2)Cl(1) 2.823(2), Sm(2)Cl(2) 2.795(2) A]. Two centroids of cyclopentadienyls two chlorine atoms, and an oxyten of THF form of a distorted trigonal bipyramid around samarium. The effective coordination number of samarium is 9.

Synthesis and structure characterization of lanthanum [2,2,2]cryptates, [LaCl[2,2,2](H2O)] Cl2 · H2O and [La(CF3SO3)[2,2,2](DMF)](CF3SO3)2

Abstract Two lanthanum(III) [2,2,2]cryptates, [LaCl[2,2,2](H2O)]Cl2 · H2O (1) and [La(CF3SO3)[2,2,2](DMF)] (CF3SO3)2 (2) have been prepared by the reaction of LaCl3 and La(CF3SO3)3 with [2,2,2]cryptand, respectively and their crystal structures have been determined. For complex 1, the La3+ ion is 10-coordinated by one chlorine ion, eight heteroatoms of a [2,2,2]cryptand and one water molecule. In the structure of complex 2, the metal ion is 10-coordinated by one monodentate CF3SO3− ion, all heteroatoms of a cryptand and a DMF molecule.

Dehydrogenation of organolanthanide alkoxides and X-ray crystal structure of reaction product [(C5H5)2 Yb(µ-OCHCCH2)]2

[Cp3Yb] reacts with HOR (Cp = C5H5; R = CH2CHCH2, CH2CH2Me) in thf (thf = tetrahydrofuran) at room temperature to give complexes [{Cp2Yb(µ-OR)}2], which are dehydrogenated to yield the new complex [{Cp2Yb(µ-OCHCCH2)}2] in refluxing thf solution; the X-ray crystal structure shows that the new complex is dimeric with oxygen atoms as bridging groups.

Synthesis and X-ray crystal structure of Sm(C8H8)(2,4-C7H11)·thf

SmCl3 reacts with K2C8H8 to yield the complex Sm(C8H8)Cl·2thf, which reacts with K(2,4-C7H11)(2,4-C7H11= 2,4-dimethylcyclopentadienyl) to form Sm(C8H8)(2,4-C7H11)·thf; the X-ray crystal structure of Sm(C8H8)(2,4-C7H11)·thf shows that the 2,4-dimethylcyclopentadienyl has a ‘U’ conformation.

Synthesis and crystal structure of [(C8H8)3(C6H5CH2C5H4)Nd2K(THF)3]

Abstract NdCl 3 reacted with C 6 H 5 CH 2 C 5 H 4 Na in the ratio 1:1 at -78°C giving [C 6 H 5 CH 2 C 5 H 4 NdCl 2 · nTHF], which then was reacted with C 8 H 8 K 2 /THF to yield the title complex [(C 8 H 8 ) 3 (C 6 H 5 CH 2 C 5 H 4 )Nd 2 K(THF) 3 ] (C 6 H 5 CH 2 C 5 H 4 = benzylcyclopentadienyl). The crystal structure of the Nd complex was determined by X-ray diffraction and revealed that the benzyl group is coordinated to the potassium atom to form a new type of trinuclear complex [(η 8 -C 8 H 8 )Nd(μ 2 -η 8 -C 8 H 8 K(THF) (η 3 -C 6 H 5 CH 2 -μ 2 — η 5 — C 5 H 4 )Nd (THF) 2 (η 8 -C 8 H 8 )]. Copyright

Synthesis and crystal structure of {[(C5H9C5H4)Er(THF)]2(μ2-Cl)3(μ3-Cl)2Na(THF)2} · THF

Abstract The reaction of ErCl3 with one equivalent of C5H9C5H4Na generates the complex {[(C5H9C5H4)Er(THF)]2(μ2-Cl)3(μ3-Cl)2Na(THF)2} · THF, which crystallizes from hexane/THF. The X-ray crystal structure determination shows that each erbium is surrounded by one C5H9C5H4 ligand, two μ3-Cl, two μ2-Cl and one THF in a distorted octahedral arrangement.

CRYSTAL-STRUCTURES OF LN(NO3)(3) (LN=EU,LU) COMPLEXES WITH A CROWN-ETHER (16-CROWN-5)

The crystal structures of Ln(NO3)(3)(Ln = Eu,Lu) complexes with 16-crown-5 are reported. In [Eu(NO3)(2)(CH3CN)(16-crown-5)][Eu(NO3)(4)(H2O)2].1/2(16-crown-5) one Eu-III ion is coordinated to two bidentate nitrate ions, one acetonitrile molecule and five o