Synthesis and structure of bis(triphenylgermane)tetrakis(tetrahydrofuran)ytterbium

A Novel Route to Triphenylgermyl Europium Complexes. Crystal Structure of (Ph3Ge)2Eu(DME)3

“…Europium naphthalene, C 10 H 8 Eu(THF) 2 , reacts with Ph 3 GeH in THF at ambient temperatures in the same way like its ytterbium analogue yielding (Ph 3 Ge) 2 Eu(THF) 4 (1 a) with about 60% yield. The conduction of the reaction in DME solution affords the corresponding complex (Ph 3 Ge) 2 Eu(DME) 3 (1 b).…”

“…; DME: 1080 and 810 cm ±1 ). Furthermore, the spectra show a weak band at 2030 cm ±1 (in [2] this band was erraneously used in proof of the formation of the hydrogen-bridged compound (Ph 3 GeH) 2 Yb(THF) 4 (3)), which may be assigned to m(Ge±H) of Ph 3 GeH formed by partial hydrolysis of the compounds during the procedure of recording.…”

“…(Ph 3 Ge) 2 Eu(DME) 3 + 2 MeI DME 2 Ph 3 GeMe + EuI 2 (DME) 2 (2) Unfortunately, all attempts failed to prepare 1 b from Ph 3 GeCl and europium metal, a route which certainly would exclude the formation of Ge±H±Eu hydrogen bridges. In contrast to the results of the reaction of Ph 3 GeCl with ytterbium metal [3], the reaction of Ph 3 GeCl with an excess of powdered europium metal in DME at room temperature proceeds only very slowly producing Ph 3 GeGePh 3 (96%) and EuCl 2 (DME) 2 (100%) as the only two products (Equ.…”

“…Ten years ago, some of us tried to synthesize a similar hydrogenbridged lanthanide complex by reacting Ph 3 GeH with ytterbium naphthalene, C 10 H 8 Yb(THF) 3 [2]. Initially, we interpreted the IR-spectroscopic data and the results of the X-ray diffraction study of the isolated diamagnetic product in the sense of the expected hydrogen-bridged complex (Ph 3 GeH) 2 Yb(THF) 4 (3). This interpretation seemed to be supported by electron density calculations as well as by the reaction of the product with dry oxygen yielding Ph 3 GeH.…”

“…Later on, a compound with just identically structural, spectroscopic and chemical properties like 3 was obtained by the reaction of Ph 3 GeCl with activated ytterbium metal [3]. However, since this synthetic route definitely excludes the formation of a hydrogen bridged compound, we recognized that the product of both reactions has to be described as (Ph 3 Ge) 2 Yb(THF) 4 (4).…”