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Stabilizing Low‐Valent Refractory Metals in a Strongly Oxidizing Medium: The First Molybdenum(V) Sulfate—MoO(HSO 4 )(SO 4 )—from Mo(CO) 6 in Oleum
Author(s) -
Betke Ulf,
Neuschulz Kai,
Wickleder Mathias S.
Publication year - 2011
Publication title -
chemistry – a european journal
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 1.687
H-Index - 242
eISSN - 1521-3765
pISSN - 0947-6539
DOI - 10.1002/chem.201101088
Subject(s) - oleum , molybdenum , thermal decomposition , refractory metals , oxidizing agent , isostructural , crystallography , decomposition , sulfate , chemistry , inorganic chemistry , materials science , crystal structure , metallurgy , organic chemistry
The reaction of Mo(CO) 6 and oleum (65 % SO 3 ) in a sealed glass tube at 200 °C leads to blue single crystals of MoO(HSO 4 )(SO 4 ). The [MoO] moieties are linked by the [SO 4 ] 2− and [HSO 4 ] − tetrahedra to form double layers that are stacked along the [100] direction (see figure). Strong hydrogen bonding is observed between the two different anions. The thermal decomposition of the compound leads, in a two‐step process, to a mixture of MoO 2 and Mo 4 O 11 .