SYNTHESIS AND STRUCTURAL CHARACTERIZATION OF K(MOO2)(PO4).H2O, AND ITS TOPOTATIC REACTION TO FORM KMOO2PO4
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abstract
K(MoO2)(PO4) H2O crystallized in the monoclinic space group P21 n with lattice parameters a = 5.846(1) , b = 8.626(1) , c = 12.364(1) , = 102.80(1), and z = 4. It was synthesized under hydrothermal conditions from a mixture of MoO3, MoO2, and K2HPO4. The structure was refined to R = 0.037 with 1223 reflections for which I > 3. Its structure consists of alternating molybdenum-oxygen octahedra and phosphate tetrahedra forming four- and eight-membered rings. The rings are connected through alternating polyhedra to form sheets. Potassium ions are located between the layers above and below the eight-membered ring. Upon heating to 500C water splits out and the layers collapse to form the three-dimensional molybdenum phosphate KMoO2PO4. This compound crystallizes in the orthorhombic space group Fddd with the cell parameters: a = 12.209(4) , b = 15.535(2) , c = 11.149(4) . The structure was determined and refined to R = 0.046 using 464 reflections with I > 3. The coalescence of layers results in a three-dimensional framework structure containing tunnels in which the K+ ions reside. 1991.