The crystal structure of a new polymorphic form of lead(II) selenite (PbSeO3) was solved
directly from conventional X-ray powder diffraction data. Direct methods and Rietveld
refinement techniques were used for the structure determination. The compound crystallizes
in the monoclinic space group P21/c (no. 14) with cell dimensions a = 9.1587(1) Å, b =
8.0902(1) Å, c = 8.7932(1) Å, β = 103.032(1)°, and V = 634.76(2) Å3. The final refinement
gave background excluded R
p = 6.22%, R
wp = 8.81%, and R
B = 2.16% by using 45 structural
and 15 profile parameters with 10 atoms in an asymmetric unit. The three-dimensional
structure consists of 9-coordinated lead atoms, which are linked by three bidentate and three
monodentate selenite groups. By combining thermal studies and X-ray powder diffraction,
the starting of irreversible phase transition between both polymorphic forms was observed,
as now reported structure transformed slowly from space group P21/c to the known structural
form P21/m between 315 and 355 °C.