The crystal structure of orthorhombic PbSO3 (Pnma, Z = 4, a = 790.3(1), b = 548.8(1), c = 680.2(1) pm) has been determined using single crystal X-ray diffraction data (final R for 663 reflections with I ≥ 2σ(I) = 0.052). The parameters of the atoms in the asymmetric unit are: Pb(4c) 0.68444(8), 0.25, 0.36072(8); S(4c) 0.5362(5), 0.25, 0.8470(5); O1(4c) 0.686(2), 0.25, 0.981(2); O2(8d) 0.563(1), 0.471(2), 0.712(1). The sulfite ion has S-O distances of 149.4(7) and 153.7(5) (twice) pm. The Pb-O

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... stances of the edge-connected Pb-O7 polyhedra (distorted mono-capped trigonal prism) range from 253.4(5) to 284.8(5) pm. The structure is closely related to that of PbSO4.