Two new coordination polymers of Pb
II complexes with bridging 4,4′‐[(1
E)‐ethane‐1,2‐diyl]bis[pyridine] (ebp), thiocyanato, and acetato ligands, [Pb(
μ‐SCN)
2(
μ‐ebp)
1.5]
n ( 1 ) and {[Pb(
μ‐OAc)(
μ‐ebp)](ClO
4)}
n ( 2 ), were synthesized and characterized by elemental analysis, FT‐IR,
1H‐ and
13C‐NMR, thermal analysis, and single‐crystal X‐ray diffraction. In 1 , the Pb
2+ ions are doubly bridged by both the ebp and the SCN
− ligands into a two‐dimensional polymeric network. The seven‐coordinate geometry around the Pb
2+ ion in 1 is a distorted monocapped trigonal prism, in which the Pb
2+ ions have a less‐common holodirected geometry. In 2 , the Pb
2+ ions are bridged by AcO
− ligands forming linear chains, which are also further bridged by the neutral ebp ligands into a two‐dimensional polymeric framework. The Pb
2+ ions have a five‐coordinate geometry with two N‐atoms from two ebp ligands and three O‐atoms of AcO
−. Although ClO acts as a counter‐ion, it also makes weak interactions with the Pb
2+ center. The arrangement of the ligands in 2 exhibits hemidirected geometry, and the coordination gap around the Pb
2+ ion is possibly occupied by a configurationally active lone pair of electrons.
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