Synthesis, magnetic susceptibility and X-ray crystal structure of (tBuNCHCHNtBu)3Yb

Autor: Richard A. Andersen, Christopher I. Dalby, F. Geoffrey N. Cloke, Phillip T. Matsunaga, Alexander A. Trifonov, Herbert Schumann, Jörg Loebel, Holger Hemling, Mikhail N. Bochkarev
Rok vydání: 1995
Předmět:
Zdroj: Journal of Organometallic Chemistry. 486:177-182
ISSN: 0022-328X
Popis: The reaction of (C 10 H 8 )Yb(THF) 3 with t BuNCHCHN t Bu ( t Budad) in tetrahydrofuran at room temperature leads to Yb( t Budad) 3 ( 1 ), which is also obtained from the reaction of YbCl 3 and three molar equivalents of K( t Budad) in tetrahydrofuran or by metal vapor synthesis. 1 has been characterized by X-ray diffraction. The crystals are monoclinic, space group C 2, Z = 2 with a = 1034.8(9), b = 1710.4(6), c = 1020.4(8) pm, β = 113.28(2)°. The structure was refined to R = 0.0274 for 1466 observed reflections ( F O > 4 σ ( F O )). The structure shows that the empirical composition is Yb( t Budad) 3 and that the coordination number of Yb is six, but the X-ray data are not sufficiently accurate to judge if the oxidation state of ytterbium is zero, two or three. The magnetic susceptibility of solid 1 , prepared by metal vapor synthesis, was studied from 5 to 300 K. The magnetic results are explained by postulating that the bivalent ytterbium species [Yb II ( t Budad)] predominates at low temperature and as the temperature increases the trivalent ytterbium species [Yb III ( t Budad − ) 3 ] predominates in the solid state.
Databáze: OpenAIRE