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Mineralogical Magazine; February 2003; v. 67; no. 1; p. 79-93; DOI: 10.1180/0026461036710086
© 2003 Mineralogical Society of Great Britain and Ireland
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The crystal structure of anthropogenic Pb2(OH)3(NO3), and a review of Pb-(O,OH) clusters and lead nitrates

U. Kolitsch* and E. Tillmanns

Institut für Mineralogie und Kristallographie, Universität Wien, Geozentrum, Althanstr. 14, A-1090 Wien, Austria

* E-mail: uwe.kolitsch{at}univie.ac.at

The previously unknown crystal structure of the basic lead nitrate Pb2(OH)3(NO3) has been determined using single-crystal X-ray diffraction data (Mo-K{alpha} radiation, CCD area detector). The compound is orthorhombic, space group Immm, with a = 8.314(2), b = 8.545(2), c = 17.210(3) Å(R1 = 2.78% for 940 ‘observed’ reflections with Fo > 4{sigma}(Fo)). The layered structure contains a previously unknown cuboid [Pb8(OH)12]4+ cluster and NO3 groups. The study used crystals formed by anthropogenic processes on a medieval mine dump, probably involving black gunpowder used in the blasting of ore. Pb2(OH)3(NO3) is associated with a second nitrate, Pb13O8(OH)6(NO3)4, which was previously designated as "Pb6O3(OH)4(NO3)2" or "Pb3(OH)5(NO3)". It is rhombohedral, space group R, with a = 10.263(1), c = 25.454(5) Å, and a structure solution is in complete agreement with an independent single-crystal study by Li et al. (2001). Probable hydrogen bonds in Pb2(OH)3(NO3) are indicated. Reported data on [Pbx2+ (O, OH)y]n+ clusters and lead hydroxide and oxide nitrates are summarized and discussed critically. The probable conditions of formation of the studied samples are evaluated.

KEYWORDS: Pb2(OH)3(NO3), lead nitrates, crystal structure, cluster, review






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