Crystal structure of antimony oxalate hydroxide, Sb(C₂O₄)OH

The crystal structure of Sb(C₂O₄)OH has been solved by charge flipping in combination with difference Fourier techniques using laboratory X-ray powder data exhibiting significant preferred orientation and refined by the Rietveld method. The compound crystallizes inPnmawitha=5.827 13(3),b=11.294 48 (10),c=6.313 77(3) Å,V=415.537(5) ų, andZ=4. The crystal structure contains pentagonal pyramidal Sb³⁺cations, which are bridged by hydroxyl groups to form zigzag chains along theaaxis. Each oxalate anion chelates to two Sb in approximately theabplane, linking the chains into a three-dimensional framework. The H of the hydroxyl group is probably disordered in order to form stronger more-linear hydrogen bonds. The highest energy occupied molecular orbitals are the Sb³⁺lone pairs. The structure is chemically reasonable compared to other antimony oxalates and to Bi(C₂O₄)OH.