ORGANOAMIDO-AND ARYLOXO-LANTHANOIDS .12. THE COORDINATION CHEMISTRY OF BIS(2-PHENYLINDOL-1-YL)YTTERBIUM(II), AND THE X-RAY CRYSTAL-STRUCTURES OF YB(PIN)(2)(DIGLYME)(THF) AND [YB(PIN)(2)(DME)](2) (PIN EQUALS 2-PHENYLINDOL-1-YL, DIGLYME EQUALS BIS(2-METHOXYETHYL)ETHER, THF EQUALS TETRAHYDROFURAN, DME EQUALS 1,2-DIMETHOXYETHANE)
Ct. Abrahams et al., ORGANOAMIDO-AND ARYLOXO-LANTHANOIDS .12. THE COORDINATION CHEMISTRY OF BIS(2-PHENYLINDOL-1-YL)YTTERBIUM(II), AND THE X-RAY CRYSTAL-STRUCTURES OF YB(PIN)(2)(DIGLYME)(THF) AND [YB(PIN)(2)(DME)](2) (PIN EQUALS 2-PHENYLINDOL-1-YL, DIGLYME EQUALS BIS(2-METHOXYETHYL)ETHER, THF EQUALS TETRAHYDROFURAN, DME EQUALS 1,2-DIMETHOXYETHANE), Australian Journal of Chemistry, 48(12), 1995, pp. 1933-1947
With the facile displacement being utilized of thf from Yb(pin)(2)(thf
)(4) (pin = 2-phenylindol-1-yl, thf = tetrahydrofuran) in toluene solu
tion, the complexes Yb(pin)(2)(dme)(2) (dme = 1,2-dimethoxyethane), Yb
(pin)(2)(tmen) (tmen = N,N,N',N'-tetramethylethane-1,2-diamine) and Yb
(pin)(2)(diglyme)(thf) (diglyme = bis(2-methoxyethyl)ether) have been
prepared from the respective ligands and Yb(pin)(2)(thf)(4). Yb(pin)(2
)(diglyme)(thf) [monoclinic, space group P2(1)/c, a 15.35(1), b 16.179
(5), c 14.45(2)Angstrom, beta 107.51(8)degrees, Z 4, R 0.044 for 2956
(I<3sigma(I)) 'observed' reflections] has a monomeric six-coordinate s
tructure with transoid nitrogen donor atoms, N-Yb-N 143.6(4)degrees an
d an irregular coordination polyhedron described as either a distorted
trigonal prism or a monocapped square pyramid. Attempted crystallizat
ion of Yb(pin)(2)(thf) by partial desolvation of Yb(pin)(2)(thf)(4) in
hot toluene, containing a trace of dme, gave a mixture of red Yb(pin)
(2)(thf) and orange[Yb(pin)(2)(dme)](2). The latter was independently
synthesized by partial desolvation of Yb(pin)(s)(dme)(2) in toluene. A
n X-ray crystal structure showed [Yb(pin)(2)(dme)](2) [monoclinic, spa
ce group P2(1)/c, a 11.614(2), b 15.945(7), c 15.327(4)Angstrom, beta
110.19(2)degrees, Z 2 dimers, R 0.070 for 2314 (I greater than or equa
l to 3sigma(I)) 'observed' reflections] to be a dimer with two bridgin
g pin ligands, coordinated through nitrogen only. There is an approxim
ately square pyramidal five-coordinate ytterbium environment with an a
pical dme oxygen, and with two bridging nitrogens, a terminal nitrogen
, and a dme oxygen in the basal plane.