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Pyrimidine-2-thione (HSpym) reacts with lead(II) thiocyanate and lead(II) bromide in N,N-dimethylformamide (DMF) to form poly[(μ-isothiocyanato-κ2N:S)(μ4-pyrimidine-2-thiolato-κ6N1,S:S:S:S,N3)lead(II)], [Pb(C4H3N2S)(NCS)]n or [Pb(Spym)(NCS)]n, (I), and the polymeric one-dimensional (1D) compound catena-poly[[μ4-bromido-di-μ-bromido-(μ-pyrimidine-2-thiolato-κ3N1,S:S)(μ-pyrimidine-2-thione-κ3N1,S:S)dilead(II)] N,N-dimethylformamide monosolvate], {[Pb2Br3(C4H3N2S)(C4H4N2S)]·C3H7NO}n or {[Pb2Br3(Spym)(HSpym)]·DMF}n, (IIa), respectively. Poly[μ4-bromido-di-μ3-bromido-(μ-pyrimidine-2-thiolato-κ3N1,S:S)(μ-pyrimidine-2-thione-κ3N1,S:S)dilead(II)], [Pb2Br3(C4H3N2S)(C4H4N2S)]n or [Pb2Br3(Spym)(HSpym)]n, (IIb), could be obtained as a mixture with (IIa) when using a lesser amount of solvent. In the crystal structures of the pseudohalide/halide PbII stable compounds, coordination of anionic and neutral HSpym has been observed. Both Spym− (in the thiolate tautomeric form) and NCS− ligands were responsible for the two-dimensional (2D) arrangement in (I). The Br− ligands establish the 1D polymeric arrangement in (IIa). Eight-coordinated metal centres have been observed in both compounds, when considering the Pb
S and Pb
Br interactions. Both compounds were characterized by FT–IR and diffuse reflectance spectroscopies, as well as by powder X-ray diffraction. Compound (IIa) and its desolvated version (IIb) represent the first structurally characterized PbII compounds containing neutral HSpym and anionic Spym− ligands. After a prolonged time in solution, (IIa) is converted to another compound due to complete deprotonation of HSpym. The structural characterization of (I) and (II) suggests HSpym as a good candidate for the removal of PbII ions from solutions containing thiocyanate or bromide ions.
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