Abstract
Single crystals of poly[μ4-tartrato-κ(6) O (1),O (3):O (1'):O (2),O (4):O (4')-lead], [Pb(C4H4O6)] n , were grown in a gel medium. In comparison with the previous structure determination of this compound from laboratory powder X-ray diffraction data [De Ridder et al. (2002 ▶). Acta Cryst. C58, m596-m598], the redetermination on the basis of single-crystal data reveals the absolute structure, all atoms with anisotropic displacement parameters and a much higher accuracy in terms of bond lengths and angles. It could be shown that a different space group or incorporation of water as reported for similarly gel-grown lead tartrate crystals is incorrect. In the structure, each Pb(2+) cation is bonded to eight O atoms of five tartrate anions, while each tartrate anion links four Pb(2+) cations. The resulting three-dimensional framework is stabilized by O-H⋯O hydrogen bonds between the OH groups of one tartrate anion and the carboxyl-ate O atoms of adjacent anions.
Highlights
Single crystals of poly[4-tartrato-6O1,O3:O1 :O2,O4:O4 -lead], [Pb(C4H4O6)]n, were grown in a gel medium
Each Pb2+ cation is bonded to eight O atoms of five tartrate anions, while each tartrate anion links four Pb2+ cations
Gel growth was the method of choice for single-crystal growth of the low-soluble fluorophosphate BaPO3F
Summary
Crystal growth in gels (Henisch, 1970) is a convenient method to obtain single crystals of high quality from compounds with rather low solubility products. Gel growth was the method of choice for single-crystal growth of the low-soluble fluorophosphate BaPO3F This compound is interesting insofar as the polycrystalline material (prepared by fast precipitation) has orthorhombic symmetry whereas single crystals grown slowly in a gel have monoclinic symmetry. After some days colourless single crystals appeared in the gel medium that, on the basis of unit-cell determinations, turned out to be lead tartrate, [Pb(C4H4O6)] The structure of this compound was originally solved and refined from laboratory. E71, 82–84 research communications (Lillybai & Rahimkutty, 2010) or in a different space group (Pna; Labutina et al, 2011) Motivated by these disagreements, it was decided to re-investigate the crystal structure of gel-grown lead tartrate on the basis of single-crystal diffraction data for an unambiguous determination of the space group and the composition, and to obtain more precise results compared to the powder refinement.
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