The new thallium(I) ortho-thiophosphates TlMPS 4 (M = Sr, Pb) were prepared applying a stoichiometric mixture of P 2 S 5 , MS, S, and Tl 2 S at high temperatures. The compound crystallizes in the orthorhombic space group Pnma and is isostructural with TlEuPS 4 [1]. It exhibits a layered structure. Each layer is composed of [(MS 6 )(TlS 6 )] n n-zigzag chains, which consist of irregular trigonal prisms alternately centred by Tl and M atoms. The layers are stacked perpendicular to the crystallographic a axis and are held together by PS 4 tetrahedra [2]. The bond valence analysis method (BVM) is used to determine where is pointing the Pb 6s 2 lone pair. (2) The phosphates were synthesized hydrothermally between 400 and 600°C at 1 kbar, using horizontally arranged Tuttle-type cold-seal bombs. The powder X-ray diffraction patterns indicate that the Cd and Mg-bearing samples are constituted by pure alluaudite for x = 0 to 1, whereas the Ca-, Ni-and Zn-bearing compounds contain small amounts of impurities. The Rietveld refinements of the powder X-ray diffraction patterns show that Cd occurs in the A(1), M(1) and M(2) sites of Na 2 CdFe 2+ Fe 3+ (PO 4 ) 3 , whereas Ca is localized in
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