Synthesis, structure and spectroscopic analyses of aquachloridooxidodiperoxidomolybdate(VI)2014 · A novel aquachloridooxidodiperoxidomolybdate(VI), [MoClO(O-2)(2)(OH2)](-), was crystallised as tetraethylammonium and triethylmethylammonium salts from strongly acidic aqueous solutions, and was structurally analysed by single crystal X-ray diffraction and NMR spectroscopy. The aqueous behaviour of the present anion observed by O-17 NMR agrees with that reported in a previous speciation study.
Potassium, rubidium and ammonium salts of -(formato-2O:O)--oxido-bis[oxidobis(peroxido-2O,O)molybdate(VI)]2013 · The unit-cell parameters of the three title salts, namely, tripotassium, K3[Mo2(CHO2)O3(O2)4], trirubidium, Rb3[Mo2(CHO2)O3(O2)4], and triammonium -(formato-2O:O)--oxido-bis[oxidobis(peroxido-2O,O)molybdate(VI)], (NH4)3[Mo2(CHO2)O3(O2)4], which were all crystallized at pH 3, are quite similar, but the potassium and rubidium salt structures are noncentrosymmetric, whereas that of the ammonium salt is centrosymmetric. Formate acts as an O:O-bridging ligand in the complex anion and is bound to a -oxido-bis(oxidodiperoxidomolybdate) unit.
Dipotassium Diaquadiphosphatooctaperoxotetramolybdate, [K-2(P2O7){MoO(O-2)(2)}(2){MoO(O-2)(2)(OH2)}(2)](2-) - a One-Dimensional Double Chain Array of Polyanions Linked by Potassium Cations2013 · A dipotassium diaquadiphosphatooctaperoxotetramolybdate, [K2(P2O7){MoO(O2)2}2{MoO(O2)2(OH2)}2]2, was crystallised as a tetramethylammonium salt and its structure was determined by single-crystal X-ray diffraction. The diaquadiphosphatooctaperoxotetramolybdate moiety (POPMo4) consists of four molybdenum decahedra and one 4-diphosphate group. All Mo atoms bear two peroxo groups at their equatorial positions. Two of the four Mo atoms are also coordinated by a water molecule. The four molybdenum decahedra are separated and linked by the diphosphate group. The POPMo4 moieties are linked by potassium atoms to form an infinite anionic 1D double chain. The chains are connected by hydrogen bonds to water of crystallisation molecules to form a 2D network. POPMo4 or its precursor gives a 31P NMR signal at = 7.3 ppm in the reaction solution and is stable at low pH and a high Mo/diphosphate molar ratio.
