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Synthesis of Double-Bridged Cofacial Nickel Porphyrin Dimers with 2,2'-Bipyridyl Pillars and Their Restricted Coordination Space. 2020

Akiharu Satake, and Yuta Katagami, and Yuki Odaka, and Yusuke Kuramochi, and Shohei Harada, and Takaya Kouchi, and Hajime Kamebuchi, and Makoto Tadokoro
Graduate School of Science, Tokyo University of Science, 1-3 Kagurazaka, Shinjuku-ku, Tokyo 162-8601, Japan.

Double-bridged cofacial Ni porphyrin dimers 2 with 2,2'-bipyridyl pillars were effectively prepared by a one-step reductive homocoupling reaction of bis(chloropyridyl)-substituted Ni porphyrin derivatives followed by a specific separation of a cyanopropyl-modified silica gel column using pyridine eluent systems. The structural analyses of 2 and its Pd complex were carried out in their solid and solution states by means of X-ray single crystal analysis and NMR, respectively. The complexation of η3-allylpalladium chloride (Pd) with 2 on the spatially restricted 2,2-bipyridine moieties on 2 gave a 2:1 (Pd:2) complex, in which the 2,2'-bipyridine ligands only provided one of the N atoms on a 2,2'-bipyridine ligand to a Pd. Therefore, the 2,2-bipyridine moieties acted as a monodentate ligand.

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