We dedicate this paper to Professor Rajeev Gupta on the occasion of his 51 st birthday.A doubly interpenetrated Cu(II)-organic framework with formula and 4,4'-bpdc = [1,1'-biphenyl]-4,4'-dicarboxylate ion) has been synthesized and characterized with the help of several spectroscopic and analytical techniques including single crystal X-ray analysis. A single crystal X-ray analysis reveals that 1 exhibit interpene-trated two-dimensional sheet-like structure containing elongated channels of cross-section 11.09 × 31.22 Å 2 along the aaxis. Finally, 1 has been exploited as a heterogeneous catalyst for the ipso-hydroxylation of arylboronic acids yielding up to 99 % of the respective phenolic product. Importantly, the catalyst can be reused for five successive cycles without having a significant loss in its catalytic efficiency.
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