ORGANOAMIDO-LANTHANOIDS AND ARYLOXO-LANTHANOIDS .10. TRIS(ETA-2-3,5-DI-T-BUTYLPYRAZOLATO)LANTHANOID(III) COMPLEXES AND THE X-RAY CRYSTAL-STRUCTURE OF ER(ETA-2-BUT2PZ)3(THF)2

被引:51
作者
COSGRIFF, JE [1 ]
DEACON, GB [1 ]
GATEHOUSE, BM [1 ]
HEMLING, H [1 ]
SCHUMANN, H [1 ]
机构
[1] TECH UNIV BERLIN,INST ANORGAN & ANALYT CHEM,D-10623 BERLIN,GERMANY
关键词
D O I
10.1071/CH9941223
中图分类号
O6 [化学];
学科分类号
0703 ;
摘要
The complexes Ln(But2pz)3(thf)2 (Ln = Y, La, Pr, Nd, Sm, Gd, Dy, Er, Yb, Lu; But2pz- = 3,5-di-t-butylpyrazolate; thf = tetrahydrofuran), and [Ln(But2pz)3(OPPh3)2].(dme). (Ln = La, n = 2/3; Ln = Er, n = 1; dme = 1,2-dimethoxyethane) have been prepared by reaction of the anthanoid metal with bis(pentafluorophenyl)mercury and the corresponding pyrazole in either thf, or 2 in dme in the presence of triphenylphosphine oxide. The X-ray crystal structure of Er(eta2-But2pz)3(thf)2 [monoclinic, space group P2(1) (No. 4), a 9.738(4), b 19.602(4), c 11.636(4) angstrom, beta 99.42(3)degrees, R 0.0374 for 3667 observed reflections] shows the complex to be an eight-coordinate monomer with three chelating But2PZ ligands. The arrangement of centres (Cen) of the N-N bonds of the But2pz ligands [<Er-N> 2.336 angstrom; Cen-Er-Cen 140.1(4)degrees, 110.3(4)degrees and 109.6(4)degrees] and the thf oxygen atoms [<Er-O> 2.351 angstrom; O-Er-O 140.1(4)degrees] is intermediate between trigonal bipyramidal and square pyramidal. The other Ln(But2pz)3(thf)2 complexes and Ln(But2pz)3(OPPh3)2 are considered to have similar structures.
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页码:1223 / 1235
页数:13
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