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Compound <jats:bold>1<\/jats:bold>, which was hydrothermally synthesized in the absence of pn ligand, exhibits the famous 2D Cairo pentagonal tiling, in which the Cu<jats:sup>I<\/jats:sup>, Cu<jats:sup>II<\/jats:sup>, and Ni<jats:sup>II<\/jats:sup> atoms act as trigonal, T\u2010shaped, and square\u2010planar nodes, respectively. Notably, there are three water molecules located at the meridianal positions of the octahedrally coordinated Cu<jats:sup>II<\/jats:sup> atom in compound <jats:bold>1<\/jats:bold>. A similar reaction, except for the addition of a small amount of pn, generated a similar Cairo pentagonal tiling layer in which two of the water molecules that were located at the meridianal positions of the octahedrally coordinated Cu<jats:sup>II<\/jats:sup> atom were replaced by a chelating pn group. Another similar hydrothermal reaction, with the addition of a larger amount of pn, yielded compound <jats:bold>3<\/jats:bold>, which showed a related two\u2010fold\u2010interpenetrated (3,4)\u2010connected 3D framework with an unprecedented {8<jats:sup>3<\/jats:sup>}<jats:sub>2<\/jats:sub>{8<jats:sup>6<\/jats:sup>} topology in which the Cu<jats:sup>II<\/jats:sup> atom was chelated by two pn groups. These structural changes between compounds <jats:bold>1<\/jats:bold>, <jats:bold>2<\/jats:bold>, <jats:bold>3<\/jats:bold> can be explained by the chelating effect of the pn group. The replacement of two meridianally coordinated water molecules on the octahedral Cu<jats:sup>II<\/jats:sup> atom in compound <jats:bold>1<\/jats:bold> by a pn group gives compound <jats:bold>2<\/jats:bold>, which shows similar Cairo tiling, and a further increase in the amount of pn results in the formation of the [Cu(NC)<jats:sub>2<\/jats:sub>(pn)<jats:sub>2<\/jats:sub>] unit and the two\u2010fold\u2010interpenetrated 3D framework of compound <jats:bold>3<\/jats:bold>. The mixed\u2010valence properties of compounds <jats:bold>1<\/jats:bold>, <jats:bold>2<\/jats:bold>, and <jats:bold>3<\/jats:bold> were confirmed by variable\u2010temperature magnetic\u2010susceptibility measurements.<\/jats:p>","DOI":"10.1002\/asia.201300143","type":"journal-article","created":{"date-parts":[[2013,4,26]],"date-time":"2013-04-26T14:56:42Z","timestamp":1366988202000},"page":"1587-1595","source":"Crossref","is-referenced-by-count":14,"title":["Heterometallic Mixed\u2010Valence Copper(I,II) Cyanides that were Tuned by Using the Chelate Effect: Discovery of Famous Cairo Pentagonal Tiling and Unprecedented (3,4)\u2010Connected {8<sup>3<\/sup>}<sub>2<\/sub>{8<sup>6<\/sup>} Topological 3D 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