A Route to Pd^o from Pd^II Metallacycles in Animation and Cross‐Coupling Chemistry

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The organic chemistry of palladacycles has been reviewed:A. D.Ryabov Synthesis1985 233.

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Crystalparameters: 0.19 × 0.27 × 0.48 mm triclinic P1(no.2) a= 9.379(1) b= 11.287(1) c= 13.573(2) Å α = 70.13(1) β = 83.68(1) γ = 69.239(9)° V= 1263.6(7) Å3 ρcalcd= 1.424 g cm−1. Data collection:T= −82°C MoKαradiation (λ = 0.71069 Å μ = 8.08 cm−1). ω‐2θ technique to a 2θmaxof 52.6°. The structure was solved by direct methods. The data were corrected for Lorentz and polarization effects but no absorption correction was applied. The hydrogen atoms were located in successive difference maps and refined isotropically. Of the 5350 (5122 unique) reflections measured 4889 that hadI> 3.00σ(I) along with 425 variable parameters were used for a full‐matrix least squares refinement. (R= Σ||Fo| ‐ |Fc||/ Σ|Fo| = 0.023 Rw= [(Σw(|Fo| ‐ |Fc|)2/ΣwF)]1/2= 0.034; min/max = −0.66 to 0.49 e−Å−3). Crystallographic data (excluding structure factors) for the structure reported in this paper have been deposited with the Cambridge Crystallographic Data Centre as supplementary publication no. CCDC‐179‐85. Copies of the data can be obtained free of charge on application to the Director CCDC 12 Union Road GB‐Cambridge CB21EZ (UK) (Fax: Int. code +(1223) 336‐033; e‐mail: [email protected]).

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We have observed some formation of Suzuki coupling products with pure catalyst1 but have not enjoyed the same high turnover numbers observed by the authors of reference [5] despite observation of Suzuki products in high yields with2. Thus our studies focus on Stille chemistry that gives high yields in our hands.