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The complex crystal structure of Bi 6 Rh 12 O 29  was determined from laboratory X-ray powder diffraction data with the software package TOPAS® [1]. The crystal symmetry is monoclinic (space group  C 2/ m ,  Z  = 4) and the unit cell parameters are  a  = 19.8510(1) Å,  b  = 12.24424(6) Å,  c  = 9.52367(5) Å and  β  = 97.2890(4)°. The structure is stable at normal pressure and room temperature. There are 4 Bi, 9 Rh and 18 O in the asymmetric unit and totally 188 atoms in the complete unit cell. Rhodium is coordinated by oxygen in slightly distorted edge sharing octahedra which build up crossing sheets both parallel (100) with a distance of  d  100 /2 and parallel (001) with a distance of  d  001 . The remaining channels along b contain the bismuth ions in irregular 6- and 8-fold coordination. Because of a small excess of oxygen in the formula – with respect to an expected amount of oxygen indicated by trivalent Bi and also trivalent Rh — the oxidation state of rhodium adjusts to a formal +3.33.

Ab initio crystal structure determination of Bi 6 Rh 12 O 29 from powder diffraction data