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

The crystal structure of Sb(C 2 O 4 )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 in Pnma with a =5.827 13(3), b =11.294 48 (10), c =6.313 77(3) A, V =415.537(5) A 3 , and Z =4. The crystal structure contains pentagonal pyramidal Sb 3+ cations, which are bridged by hydroxyl groups to form zigzag chains along the a axis. Each oxalate anion chelates to two Sb in approximately the ab plane, 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 Sb 3+ lone pairs. The structure is chemically reasonable compared to other antimony oxalates and to Bi(C 2 O 4 )OH.