Several calixdiquinone–lead(II) complexes have been prepared. Two momonomeric complexes have been prepared with p-tert-butyl-(26,28-crown-5)calixdiquinone L1 and p-tert-butylcalixdiquinone bis(ethyl ether)L2, namely [PbL1(ClO4)2] and [PbL2(ClO4)2(H2O] wherein the metal atoms are 10-coordinate being bonded to the four oxygen atoms at the lower rim of the calixdiquinone and three perchlorate oxygen atoms together with three crown oxygen atoms or two carbonyl oxygen atoms and a water molecule respectively. <br/>By contrast the lead(II) complex with calixdiquinone bis(acid)L3 forms a unique trimeric [Pb9(L3– 2H)3(ClO4)6(OH)6] unit with crystallographic 3/m symmetry containing three unique Pb(II) atoms. One of these is to be found within the calixdiquinone bonded to the four oxygen atoms at the lower rim, two acid oxygen atoms, two perchlorate anions and a water molecule. The other two Pb(II) atoms are bonded to carbonylic oxygen atoms, water molecules and hydroxide ions. These trimeric units are interconnected via upper rim quinone oxygen–Pb(II) interactions to form a three-dimensional network containing channels of ca. 14 Å in diameter
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