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Synthesis of novel lead–molybdenum and lead–tungsten oxyhalides with the pinalite structure, Pb₃MoO₅Cl₂ and Pb₃WO₅Br₂

¹ Department of Materials Sciences, Moscow State University, Leninskie Gory, Moscow 119992, Russia
² EaStChem, School of Chemistry, St. Andrews University, St. Andrews, KY16 9ST, U.K.

Correspondence: ^* E-mail: charkin{at}inorg.chem.msu.ru

Two new quaternary lead oxyhalides, Pb₃MoO₅Cl₂ and Pb₃WO₅Br₂, have been prepared. They are isostructural with the mineral pinalite, Pb₃WO₅Cl₂, and its barium analog. The crystal structure of Pb₃MoO₅Cl₂ has been refined from powder neutron diffraction data to R_p = 0.0564 and R_wp = 0.0342. All these structures contain significantly stretched MO₅ (M = Mo, W) square pyramids incorporated into the [Pb₂O₂] sheets. Bond valence sums indicate significant overbonding of one of the metal sites, which increases along with structural distortions when passing from Pb₃MoO₅Cl₂ to Pb₃WO₅Cl₂ and from Pb₃WO₅Cl₂ to Ba₃WO₅Cl₂. Possibilities of preparing isostructural and structurally related compounds are discussed.

Key Words: Pb₃MoO₅Cl₂ • pinalite • crystal structure • neutron diffraction