Hexa- To Octamolybdate Rearrangement Leads To The New Coordination Polymer [Ag(Phcn)(Thb)](4)[Beta-Mo8o26](Phcn)(2)

Polyoxomolybdates tend to re-agglomerate to -octamolybdate upon reaction with Ag+ under hydrothermal conditions and in organic solvents. Consistent with this tendency, a new coordination polymer [Ag(PhCN)(thb)](4)[-Mo8O26](PhCN)(2) (thb = theobromine) (1) was obtained and characterized by single crystal XRD, powder XRD, DTA/TG, IR, UV/Vis, and elemental analysis. 1 is a one-dimensional coordination polymer, in which octamolybdate anions are joined by [Ag(PhCN)(thb)](+) cations along the crystallographic a axis. A firm network of intermolecular interactions, especially between self-pairing thb ligands, interlinks these chains. Salt 1 is turned into MoO2 and Ag upon thermolysis in an intramolecular redox reaction.