Synthesis and Structural
Characterization of Metallogermylenes,
Cp-Substituted Germylene, and a Germanium(II)-Borane Adduct from Pyridyl-1-azaallyl
Germanium(II) Chloride
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Abstract
The reaction of [{N(SiMe<sub>3</sub>)C(Ph)C(SiMe<sub>3</sub>)(C<sub>5</sub>H<sub>4</sub>N-2)}GeCl] (<b>1</b>) with
Na[M(η<sup>5</sup>-C<sub>5</sub>H<sub>5</sub>)(CO)<sub>3</sub>]·2DME (M
= Mo, W) afforded the metallogermylenes [{N(SiMe<sub>3</sub>)C(Ph)C(SiMe<sub>3</sub>)(C<sub>5</sub>H<sub>4</sub>N-2)}Ge-M(η<sup>5</sup>-C<sub>5</sub>H<sub>5</sub>)(CO)<sub>3</sub>] (M = Mo (<b>2</b>),
W (<b>3</b>)). Compounds <b>2</b> and <b>3</b> have
been characterized by X-ray crystallography and NMR and IR spectroscopy.
Structural analyses of compounds <b>2</b> and <b>3</b> are consistent with the presence of lone-pair electrons at the germanium(II)
center. The Ge–Mo and Ge–W bond distances of 2.875(1)
and 2.852(1) Å are consistent with Ge–metal single bonds.
The chlorogermylene <b>1</b> was also used in the synthesis
of a substituted germylene, [{N(SiMe<sub>3</sub>)C(Ph)C(SiMe<sub>3</sub>)(C<sub>5</sub>H<sub>4</sub>N-2)}Ge(η<sup>1</sup>-C<sub>5</sub>H<sub>5</sub>)] (<b>4</b>), by reaction with sodium cyclopentadienylide.
The reaction of compound <b>1</b> with tris(pentafluorophenyl)borane
led to the formation of a Lewis acid–base adduct, [{N(SiMe<sub>3</sub>)C(Ph)C(SiMe<sub>3</sub>)(C<sub>5</sub>H<sub>4</sub>N-2)}Ge(Cl)→B(C<sub>6</sub>F<sub>5</sub>)<sub>3</sub>] (<b>5</b>)
