A complex isolated from a mixture of tetrasodium 5, 11, 17, 23-tetrasulfonatocalix arene-25, 26, 27, 28-tetrol and Mn(II) has been analyzed by X-ray crystallography. The crystal packing diagram featured a clay-like bilayer structure as reported previously for the analogous crystals. Interestingly, Mn(II) ions present in the hydrophilic layer cross-link two hydrophobic layers through coordination to the sulfonato groups. Because of this complex formation the repeat unit of the layer (12.1 A) is shorter than those for analogous systems (13.7-15.0 A).The structure features a Mn(II)-bridged biscalixarene with a large inner cavity. X-Ray crystallographic and ESR spectral data show that Mn(II) ions adopt a distorted octahedral coordination geometry with two sulfonato groups occupying the cis coordination. This is a novel coordination mode for a metal-bridged biscalixarene in the solid state.
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