Synthesis and characterization of the 'Japanese rice-ball'-shaped molybdenum blue Na<sub>4</sub>[Mo<sub>2</sub>O<sub>2</sub>(OH)<sub>4</sub>(C<sub>6</sub>H<sub>4</sub>NO<sub>2</sub>)<sub>2</sub>]<sub>2</sub>[Mo<sub>120</sub>Ce<sub>6</sub>O<sub>366</sub>H<sub>12</sub>(OH)<sub>2</sub>(H<sub>2</sub>O)<sub>76</sub>]~200H<sub>2</sub>O
- Author(s)
- Emir Al-Sayed, Elias Tanuhadi, Gerald Giester, Annette Rompel
- Abstract
The hybridized lanthanide-containing molybdenum blue (Ln-MB) wheel Na4[Mo2O2(OH)4(C6H4NO2)2]2[Mo120Ce6O366H12(OH)2(H2O)76]∼200H2O ({Mo2(C6H4NO2)2}2{Mo120Ce6}) was assembled in an aqueous one-pot synthesis. The Ln-MB was hybridized with 2-picolinic acid through the generation of the organometallic counter-ion [Mo2O2(OH)4(C6H4NO2)2]2+. Control experiments demonstrated that the position of the carboxylic acid group (2-position to the N atom) in the hybridization component is critical in yielding single crystals of Ln-MB. In addition to single-crystal X-ray diffraction (XRD) analysis, which revealed a `Japanese rice-ball'-shaped Ln-MB as the anion, elemental analyses, IR spectroscopy, and thermogravimetric analysis (TGA) were performed to confirm its structure and composition. Bond-valence-sum calculations (BVS) revealed that {Mo2(C6H4NO2)2}2{Mo120Ce6} is composed of a 24-electron reduced anionic ring, which was confirmed by Vis–NIR spectroscopy.
- Organisation(s)
- Department of Biophysical Chemistry, Department of Mineralogy and Crystallography
- Journal
- Acta Crystallographica. Section C: Structural Chemistry
- Volume
- 78
- Pages
- 299-304
- No. of pages
- 6
- ISSN
- 2053-2296
- DOI
- https://doi.org/10.1107/S2053229622003369
- Publication date
- 05-2022
- Peer reviewed
- Yes
- Austrian Fields of Science 2012
- 105116 Mineralogy, 104017 Physical chemistry, 105113 Crystallography
- Keywords
- ASJC Scopus subject areas
- Condensed Matter Physics, Materials Chemistry, Inorganic Chemistry, Physical and Theoretical Chemistry
- Portal url
- https://ucrisportal.univie.ac.at/en/publications/f28c89e8-b929-456c-978c-37a7579f773a