(Acetato-κ2 O,O′)[2′-(di-tert-butylphosphanyl)-1,1′-biphenyl-κ2 P,C 2]palladium(II)

The structure of the title compound, [Pd(C2H3O2)(C20H26P)], shows a distorted square-planar geometry for the PdII atom, with significant deviations being evident owing to the asymmetric coordination mode of the acetate ligand. A weak intramolecular C—H⋯O interaction is noted. The crystal studied was a racemic twin.

The structure of the title compound, [Pd(C 2 H 3 O 2 )(C 20 H 26 P)], shows a distorted square-planar geometry for the Pd II atom, with significant deviations being evident owing to the asymmetric coordination mode of the acetate ligand. A weak intramolecular C-HÁ Á ÁO interaction is noted. The crystal studied was a racemic twin.
There is significant deviation from the ideal square planar geometry around the Pd atom as a result of its coordination to the acetate moiety. This distorted geometry is evident from the deviations in bond angles from 90°. The data in Table 1 demonstrate the deviations in the coordination geometry. A weak intramolecular C-H···O interaction is noted ( Fig. 2 and Table 2).

Experimental
A solution of 2-(biphenyl)-di-tert-butylphosphine (298 mg; 1 mmol) and palladium acetate (224 mg; 1 mmol) in 15 ml of chloroform was refluxed under argon for 3 h. The solvent was evaporated in vacuo to leave a colourless crystalline residue (464 mg; ca 100%). The solid was taken up in dichloromethane (3 ml) and the solution diluted with cyclohexane (10 ml). The solvent was allowed to slowly evaporate in a stream of nitrogen until the solution was reduced to 3 ml. This resulted in the formation of well formed yellow blocks of the title compound (I) (288 mg; m.p. 409-414 K).

Refinement
The H atoms were included at idealized positions and were allowed to ride with C-H = 0.95-0.98 Å, and with U iso (H) = 1.2-1.5U eq (C). The structure was refined as a racemic twin precluding the determination of the absolute structure. Owing to poor agreement, the 0 1 6 and 1 4 0 reflections were omitted from the final refinement.

Crystal data
[Pd(C 2 H 3 O 2 )(C 20 H 26 P)] M r = 462.82 Orthorhombic, P2 1 2 1 2 1 Hall symbol: P 2ac 2ab a = 9.800 (3)    Refinement. Refinement of F 2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F 2 , conventional R-factors R are based on F, with F set to zero for negative F 2 . The threshold expression of F 2 > σ(F 2 ) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F 2 are statistically about twice as large as those based on F, and R-factors based on ALL data will be even larger.