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Coletta, Marco
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article
With complements of the ligands: an unusual S-shaped [Mn7]2 assembly from tethered calixarenes
Abstract
The reaction between MnCl<sub>2</sub>·4H<sub>2</sub>O, 2,2′-bis-<i>p</i>-<sup>t</sup>Bu-calix[4]arene (H<sub>8</sub>L1) and 2-(hydroxymethyl)pyridine (hmpH) in a basic dmf/MeOH solution results in the formation of the complex [Mn<sup>III</sup><sub>10</sub>Mn<sup>II</sup><sub>4</sub>(L1)<sub>3</sub>(hmp)<sub>4</sub>(μ<sub>3</sub>-O)<sub>4</sub>(μ<sub>3</sub>-OH)<sub>2</sub>(MeOH)<sub>4</sub>(dmf)<sub>6</sub>](dmf)<sub>4</sub> (<b>6</b>) upon vapour diffusion of petroleum ether into the mother liquor. The crystals are in the monoclinic space group <i>C</i>2/<i>c</i>, with the asymmetric unit (ASU) comprising one half of the molecule. The structure describes a large <i>S</i>-shaped cluster (∼40 Å top to tail) where the unusual syn and anti conformations of the calixarene ligands results in two binding pockets each containing a [Mn<sup>III</sup><sub>5</sub>Mn<sup>II</sup><sub>2</sub>] moiety comprised of two perpendicular, vertex-sharing [Mn<sub>4</sub>] butterflies. One butterfly possesses a [Mn<sup>III</sup><sub>4</sub>O<sub>4</sub>] core and the second a [Mn<sup>III</sup><sub>2</sub>Mn<sup>II</sup><sub>2</sub>O<sub>3</sub>] unit with the Mn<sup>II</sup> ions in the central body positions. Magnetic susceptibility and magnetisation measurements reveal weak exchange interactions between the metal centres.