A one-pot procedure has been developed for the direct and atom-economical preparation of the pincertype complexes 3, 2 ). This convenient synthetic protocol involves heating a 1 : 2 : 1-2 mixture of resorcinol (or its substituted derivatives), R 2 PCl, and nickel powder in toluene (at 100 °C) or acetonitrile (at 75 °C) for 18 h. The target nickel compounds can be obtained from this procedure in up to 93% yield.Using metallic palladium in this protocol instead of nickel gives the corresponding palladium complexes in low yields only (ca. 10%).
Chart 1Scheme 1 † Electronic supplementary information (ESI) available: Tables of crystal dataand collection/refinement parameters. Complete details of the X-ray analyses. CCDC 928921 (2), 928922 (3) and 928920 (4). For ESI and crystallographic data in CIF or other electronic format see
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