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Crystal chemistry of basic lead carbonates. III. Crystal structures of Pb₃O₂(CO₃) and NaPb₂(OH)(CO₃)₂

S. V. Krivovichev^*, and P. C. Burns

Department of Civil Engineering and Geological Sciences, 156 Fitzpatrick, University of Notre Dame, Notre Dame IN 46556-0767 USA

^* E-mail: sergey{at}cryst.geol.pu.ru

The crystal structures of synthetic Pb₃O₂(CO₃) and NaPb₂(OH)(CO₃)₂, have been solved by direct methods and refined to R = 0.062 and 0.024, respectively. Pb₃O₂(CO₃) is orthorhombic, Pnma, a = 22.194(3), b = 9.108(1), c = 5.7405(8) Å, V = 1160.4(3) ų, Z = 8. There are four symmetrically distinct Pb²⁺ cations in irregular coordination polyhedra due to the effect of stereoactive s² lone-electron pairs. The structure is based upon double [O₂Pb₃] chains of [O(1)Pb₄] and [O(2)Pb₄] oxocentred tetrahedra and CO₃ groups. The [O₂Pb₃] chains are parallel to the c axis, whereas the CO₃ groups are parallel to the (010) plane. NaPb₂(OH)(CO₃)₂ is hexagonal, P6₃mc, a = 5.276(1), c = 13.474(4) Å, V = 324.8(1) ų, Z = 2 and has been solved by direct methods. There are two symmetrically distinct Pb²⁺ cations in asymmetric coordination polyhedra due to the effect of stereoactive s² lone-electron pairs. The single symmetrically unique Na⁺ cation is in trigonal prismatic coordination. The structure is based on hexagonal sheets of Pb atoms. Within these sheets, Pb atoms are located at vertices of a 3⁶ net, such that each Pb atom has six adjacent Pb atoms that are ~5.3 Åaway. Two sheets are stacked in a close-packing arrangement, forming layers that contain the (CO₃) groups. The layers are linked by OH groups that are linearly coordinated by two Pb²⁺ cations. Na⁺ cations are located between the layers. The structure is closely related to the structures of other lead hydroxide carbonates (leadhillite, macphersonite, susannite, hydrocerussite, ‘plumbonacrite’).

KEYWORDS: basic lead carbonates, lone-electron pairs, oxocentred tetrahedra, hexagonal lead sublattice

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