Dicarbonyl-1κ2C-μ-chlorido-2:3κ2Cl:Cl-pentachlorido-2κ2Cl,3κ3Cl-[1(η6)-toluene]digallium(III)ruthenium(I)(Ru—Ga)

The title compound is a ruthenium–gallium metal cluster. The ruthenium and gallium have a direct metal–metal bond with a length of 2.4575 (2) Å.

The Ru1-Ga1 bond length of 2.4575 (2) A ˚for the title compound is very similar to the value of 2.453 (1) A ˚observed for Ru 2 {GaCl 2 (THF)} 2 (CO) 8 (Harakas & Whittlesey, 1997).The packing is shown in Fig. 2 During the work-up of the reaction, the title compound was isolated directly from the toluene solution.It is unknown at this time the role of diphenylsilanediol, if any, in the formation of the title compound.A solid that was insoluble in toluene in the reaction flask was extracted with THF forming an orange solution.This reaction product, which may contain the desired diphenylsiloxane metal cluster, has not yet been fully characterized.

Synthesis and crystallization
All manipulations were carried out under argon using standard Schlenk line techniques.Our previous work (Demmin et al., 2024) demonstrated that silicone-based vacuum grease can contaminate gallium halide reactions.Therefore, PTFE sleeves and non-silicone based vacuum grease were used on all glassware in this experiment.In a 250 ml Schlenk flask, gallium (5.60 g, 80.3 mmole) and GaCl 3 5.00 g (28.4,mmole) were combined followed by toluene (175 ml).The mixture was heated to reflux for 24 h to produce a solution containing gallium(II) chloride (Ga 2 Cl 4 ), excess gallium was present.
Diphenylsilanediol (0.306 g, 1.41 mmol) was added to a 150 ml Schlenk flask followed by toluene (50 ml).To this flask, 10 ml of the Ga 2 Cl 4 stock solution was added via cannula.The dark-gray mixture was refluxed under argon for 72 h resulting in a light-gray mixture.The reaction flask was cooled to 25 � C and Ru 3 (CO) 12 (0.225 g, 0.352 mmol) was then added.The mixture was heated to reflux for an additional 72 h.This resulted in a mixture with a suspended gray solid/gel and colorless solution.The colorless solution was decanted into a 150 ml Schlenk flask via cannula.After standing at 25 � C for 10 days, colorless crystals were observed.
A single crystal was coated with NVH oil and mounted on a MiTeGen loop under a stream of argon gas then cooled to À 25 � C for data collection.

Figure 1
The molecular structure of the title compound.Displacement ellipsoids are drawn at the 50% probability level.

Figure 2
Crystal packing diagram viewed along the b axis.Hydrogen atoms have been omitted for clarity.

Special details
Geometry.All esds (except the esd in the dihedral angle between two l.s.planes) are estimated using the full covariance matrix.The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry.An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s.planes.Geometric parameters (Å, º) Smith and Harakas � [RuGa 2 Cl 6 (C 7 H 8 )(CO) 2 ]IUCrData (2024).9, x240657

Table 2
Experimental details.