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Mo2Bi28O47 crystallizes in the triclinic P1 space group. The structure is three-dimensional. there are two inequivalent Mo5+ sites. In the first Mo5+ site, Mo5+ is bonded to four O2- atoms to form MoO4 tetrahedra that share a cornercorner with one BiO6 octahedra. The corner-sharing octahedral tilt angles are 45°. There are a spread of Mo–O bond distances ranging from 1.79–1.81 Å. In the second Mo5+ site, Mo5+ is bonded in a trigonal planar geometry to three O2- atoms. There are a spread of Mo–O bond distances ranging from 1.81–1.90 Å. There are twenty-eight inequivalent Bi3+ sites. In the first Bi3+ site, Bi3+ is bonded in a 6-coordinate geometry to six O2- atoms. There are a spread of Bi–O bond distances ranging from 2.14–3.00 Å. In the second Bi3+ site, Bi3+ is bonded to five O2- atoms to form distorted corner-sharing BiO5 square pyramids. There are a spread of Bi–O bond distances ranging from 2.11–2.70 Å. In the third Bi3+ site, Bi3+ is bonded in a distorted body-centered cubic geometry to eight O2- atoms. There are a spread of Bi–O bond distances ranging from 2.32–2.91 Å. In the fourth Bi3+ site, Bi3+ is bonded in a 6-coordinate geometry to six O2- atoms. There are a spread of Bi–O bond distances ranging from 2.16–2.80 Å. In the fifth Bi3+ site, Bi3+ is bonded in a 6-coordinate geometry to six O2- atoms. There are a spread of Bi–O bond distances ranging from 2.24–2.84 Å. In the sixth Bi3+ site, Bi3+ is bonded in a 6-coordinate geometry to six O2- atoms. There are a spread of Bi–O bond distances ranging from 2.14–2.96 Å. In the seventh Bi3+ site, Bi3+ is bonded to six O2- atoms to form distorted edge-sharing BiO6 octahedra. There are a spread of Bi–O bond distances ranging from 2.20–2.71 Å. In the eighth Bi3+ site, Bi3+ is bonded in a 5-coordinate geometry to five O2- atoms. There are a spread of Bi–O bond distances ranging from 2.13–2.70 Å. In the ninth Bi3+ site, Bi3+ is bonded to five O2- atoms to form distorted corner-sharing BiO5 square pyramids. There are a spread of Bi–O bond distances ranging from 2.12–2.63 Å. In the tenth Bi3+ site, Bi3+ is bonded in a 6-coordinate geometry to six O2- atoms. There are a spread of Bi–O bond distances ranging from 2.26–2.84 Å. In the eleventh Bi3+ site, Bi3+ is bonded in a 6-coordinate geometry to six O2- atoms. There are a spread of Bi–O bond distances ranging from 2.15–2.95 Å. In the twelfth Bi3+ site, Bi3+ is bonded in a distorted body-centered cubic geometry to eight O2- atoms. There are a spread of Bi–O bond distances ranging from 2.36–2.79 Å. In the thirteenth Bi3+ site, Bi3+ is bonded in a distorted body-centered cubic geometry to eight O2- atoms. There are a spread of Bi–O bond distances ranging from 2.33–2.84 Å. In the fourteenth Bi3+ site, Bi3+ is bonded in a 5-coordinate geometry to five O2- atoms. There are a spread of Bi–O bond distances ranging from 2.13–2.73 Å. In the fifteenth Bi3+ site, Bi3+ is bonded in a 7-coordinate geometry to seven O2- atoms. There are a spread of Bi–O bond distances ranging from 2.29–2.83 Å. In the sixteenth Bi3+ site, Bi3+ is bonded in a 6-coordinate geometry to six O2- atoms. There are a spread of Bi–O bond distances ranging from 2.26–2.86 Å. In the seventeenth Bi3+ site, Bi3+ is bonded in a 5-coordinate geometry to five O2- atoms. There are a spread of Bi–O bond distances ranging from 2.14–2.77 Å. In the eighteenth Bi3+ site, Bi3+ is bonded in a 6-coordinate geometry to six O2- atoms. There are a spread of Bi–O bond distances ranging from 2.14–3.02 Å. In the nineteenth Bi3+ site, Bi3+ is bonded in a 6-coordinate geometry to six O2- atoms. There are a spread of Bi–O bond distances ranging from 2.14–2.99 Å. In the twentieth Bi3+ site, Bi3+ is bonded to six O2- atoms to form distorted BiO6 octahedra that share a cornercorner with one BiO6 octahedra and a cornercorner with one MoO4 tetrahedra. The corner-sharing octahedral tilt angles are 49°. There are a spread of Bi–O bond distances ranging from 2.15–2.90 Å. In the twenty-first Bi3+ site, Bi3+ is bonded in a 6-coordinate geometry to six O2- atoms. There are a spread of Bi–O bond distances ranging from 2.27–2.84 Å. In the twenty-second Bi3+ site, Bi3+ is bonded in a 6-coordinate geometry to six O2- atoms. There are a spread of Bi–O bond distances ranging from 2.28–2.85 Å. In the twenty-third Bi3+ site, Bi3+ is bonded to six O2- atoms to form a mixture of distorted edge and corner-sharing BiO6 octahedra. The corner-sharing octahedral tilt angles are 49°. There are a spread of Bi–O bond distances ranging from 2.17–2.85 Å. In the twenty-fourth Bi3+ site, Bi3+ is bonded in a distorted body-centered cubic geometry to eight O2- atoms. There are a spread of Bi–O bond distances ranging from 2.34–2.82 Å. In the twenty-fifth Bi3+ site, Bi3+ is bonded in a 7-coordinate geometry to seven O2- atoms. There are a spread of Bi–O bond distances ranging from 2.26–2.89 Å. In the twenty-sixth Bi3+ site, Bi3+ is bonded in a 5-coordinate geometry to five O2- atoms. There are a spread of Bi–O bond distances ranging from 2.16–2.75 Å. In the twenty-seventh Bi3+ site, Bi3+ is bonded in a 6-coordinate geometry to six O2- atoms. There are a spread of Bi–O bond distances ranging from 2.14–3.12 Å. In the twenty-eighth Bi3+ site, Bi3+ is bonded in a 7-coordinate geometry to seven O2- atoms. There are a spread of Bi–O bond distances ranging from 2.28–2.87 Å. There are forty-seven inequivalent O2- sites. In the first O2- site, O2- is bonded in a distorted single-bond geometry to one Mo5+ and one Bi3+ atom. In the second O2- site, O2- is bonded in a 4-coordinate geometry to four Bi3+ atoms. In the third O2- site, O2- is bonded to four Bi3+ atoms to form a mixture of edge and corner-sharing OBi4 tetrahedra. In the fourth O2- site, O2- is bonded to four Bi3+ atoms to form a mixture of edge and corner-sharing OBi4 tetrahedra. In the fifth O2- site, O2- is bonded in a 4-coordinate geometry to four Bi3+ atoms. In the sixth O2- site, O2- is bonded in a 4-coordinate geometry to four Bi3+ atoms. In the seventh O2- site, O2- is bonded in a 4-coordinate geometry to four Bi3+ atoms. In the eighth O2- site, O2- is bonded in a 4-coordinate geometry to four Bi3+ atoms. In the ninth O2- site, O2- is bonded in a 4-coordinate geometry to four Bi3+ atoms. In the tenth O2- site, O2- is bonded to four Bi3+ atoms to form a mixture of edge and corner-sharing OBi4 tetrahedra. In the eleventh O2- site, O2- is bonded to four Bi3+ atoms to form a mixture of edge and corner-sharing OBi4 tetrahedra. In the twelfth O2- site, O2- is bonded in a 4-coordinate geometry to four Bi3+ atoms. In the thirteenth O2- site, O2- is bonded in a 4-coordinate geometry to four Bi3+ atoms. In the fourteenth O2- site, O2- is bonded to four Bi3+ atoms to form a mixture of edge and corner-sharing OBi4 tetrahedra. In the fifteenth O2- site, O2- is bonded to four Bi3+ atoms to form a mixture of edge and corner-sharing OBi4 tetrahedra. In the sixteenth O2- site, O2- is bonded to four Bi3+ atoms to form a mixture of edge and corner-sharing OBi4 tetrahedra. In the seventeenth O2- site, O2- is bonded in a 4-coordinate geometry to four Bi3+ atoms. In the eighteenth O2- site, O2- is bonded to four Bi3+ atoms to form a mixture of edge and corner-sharing OBi4 tetrahedra. In the nineteenth O2- site, O2- is bonded in a 4-coordinate geometry to four Bi3+ atoms. In the twentieth O2- site, O2- is bonded in a 4-coordinate geometry to four Bi3+ atoms. In the twenty-first O2- site, O2- is bonded in a 4-coordinate geometry to four Bi3+ atoms. In the twenty-second O2- site, O2- is bonded in a 4-coordinate geometry to four Bi3+ atoms. In the twenty-third O2- site, O2- is bonded in a 4-coordinate geometry to four Bi3+ atoms. In the twenty-fourth O2- site, O2- is bonded in a distorted single-bond geometry to one Mo5+ and four Bi3+ atoms. In the twenty-fifth O2- site, O2- is bonded in a 4-coordinate geometry to four Bi3+ atoms. In the twenty-sixth O2- site, O2- is bonded to four Bi3+ atoms to form a mixture of edge and corner-sharing OBi4 tetrahedra. In the twenty-seventh O2- site, O2- is bonded in a 4-coordinate geometry to four Bi3+ atoms. In the twenty-eighth O2- site, O2- is bonded to four Bi3+ atoms to form a mixture of edge and corner-sharing OBi4 tetrahedra. In the twenty-ninth O2- site, O2- is bonded to four Bi3+ atoms to form a mixture of edge and corner-sharing OBi4 tetrahedra. In the thirtieth O2- site, O2- is bonded to four Bi3+ atoms to form a mixture of edge and corner-sharing OBi4 tetrahedra. In the thirty-first O2- site, O2- is bonded in a 4-coordinate geometry to four Bi3+ atoms. In the thirty-second O2- site, O2- is bonded in a 4-coordinate geometry to four Bi3+ atoms. In the thirty-third O2- site, O2- is bonded to four Bi3+ atoms to form a mixture of edge and corner-sharing OBi4 tetrahedra. In the thirty-fourth O2- site, O2- is bonded to four Bi3+ atoms to form a mixture of edge and corner-sharing OBi4 tetrahedra. In the thirty-fifth O2- site, O2- is bonded in a 4-coordinate geometry to four Bi3+ atoms. In the thirty-sixth O2- site, O2- is bonded in a 2-coordinate geometry to one Mo5+ and two Bi3+ atoms. In the thirty-seventh O2- site, O2- is bonded in a 4-coordinate geometry to four Bi3+ atoms. In the thirty-eighth O2- site, O2- is bonded in a 4-coordinate geometry to four Bi3+ atoms. In the thirty-ninth O2- site, O2- is bonded in a 1-coordinate geometry to one Mo5+ and two Bi3+ atoms. In the fortieth O2- site, O2- is bonded in a 4-coordinate geometry to four Bi3+ atoms. In the forty-first O2- site, O2- is bonded in a distorted single-bond geometry to one Mo5+ and one Bi3+ atom. In the forty-second O2- site, O2- is bonded in a 4-coordinate geometry to four Bi3+ atoms. In the forty-third O2- site, O2- is bonded to four Bi3+ atoms to form a mixture of edge and corner-sharing OBi4 tetrahedra. In the forty-fourth O2- site, O2- is bonded to four Bi3+ atoms to form a mixture of edge and corner-sharing OBi4 tetrahedra. In the forty-fifth O2- site, O2- is bonded in a 4-coordinate geometry to four Bi3+ atoms. In the forty-sixth O2- site, O2- is bonded in a distorted single-bond geometry to one Mo5+ and two Bi3+ atoms. In the forty-seventh O2- site, O2- is bonded in a 2-coordinate geometry to one Mo5+ and one Bi3+ atom.

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