| Summary: | Mixed-ligand lead(II) complexes with 2,2′-bipyridyl and [B<sub>10</sub>H<sub>9</sub>OH]<sup>2−</sup> or monosubstituted hydroxy-substituted <i>closo</i>-decaborate anions with a pendant hydroxy group, separated from the boron cage by an alkoxylic spacer of different lengths [B<sub>10</sub>H<sub>9</sub>O(CH<sub>2</sub>)<i><sub>x</sub></i>O(CH<sub>2</sub>)<sub>2</sub>OH]]<sup>2−</sup> (<i>x</i> = 2 or 5) have been synthesized. Compounds have been characterized by IR and multinuclear NMR spectroscopies. The structures of binuclear complex [Pb(bipy)<sub>2</sub>[B<sub>10</sub>H<sub>9</sub>OH]]<sub>2</sub>·CH<sub>3</sub>CN (<b>1</b>·CH<sub>3</sub>CN), mononuclear complex [Pb(bipy)<sub>2</sub>[B<sub>10</sub>H<sub>9</sub>O(CH<sub>2</sub>)<sub>2</sub>O(CH<sub>2</sub>)<sub>2</sub>OH]]·0.5bipy·CH<sub>3</sub>CN (<b>2</b>·0.5bipy·CH<sub>3</sub>CN), and polymeric complex [Pb(bipy)[B<sub>10</sub>H<sub>9</sub>O(CH<sub>2</sub>)<sub>5</sub>O(CH<sub>2</sub>)<sub>2</sub>OH]]<i><sub>n</sub></i> (<b>3</b>) have been determined by single-crystal X-ray diffraction. In all three compounds, the co-ordination polyhedra of lead(II) are formed by N atoms from two bipy molecules, O atoms of the substituent attached to the boron cage, and BH groups of the boron cage.
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