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