Hydrothermal Synthesis and Crystal Structure of a New Sandwich—type Molybdenum Phosphate

1 INTRODUCTION The synthesis of porous and open-framework transition metal phosphates has received great in- terest due to their various compositions and topolo- gyies, as well as their useful properties such as con- trollable size- and shape-selectivity, rigid frame- works and chemical/thermal stability1]. Of these phosphates constructed from oxometal polyhedra and PO4 tetrahedron, the most interesting is the MoV6P4X31]n－ (X=O, OH) family with the dimen- sionalities ranging from …

Hydrothermal Synthesis and Crystal Structure of a New Sandwich-type Molybdenum Phosphate

The crystal structure of the title compound, enH2]Fe{MoV6O12(OH)3(HPO4)-(H2PO4)3}2].6en.6H2O (en = H2NCH2CH2NH2), hydrothermally synthesized from a mixture of Na2MoO4@2H2O, Fe2(SO4)3, H3PO4, H2N(CH2)2NH2 and water, has been determined by singlecrystal X-ray diffraction. The crystal is of triclinic, space group P1- with a = 11.9014(1), b =13.4246(2), c = 13.8719(2) A, α= 87.465(1), β= 69.981(1), γ= 64.960(1)°, V= 1873.46(4) A3, Z=1, Mr = 2997.89, F(000) = 1466,μ = 2.427 mm-1 and Dc = 2.657 g/cm3. The final R = 0.0404 for 5570 observed reflections (Ⅰ＞ 2σ(Ⅰ)). The structural analysis reveals that each cluster anion contains two coplanar {Mo6} rings of six edge-sharing Mo(O5OH) octahedra, and the two {Mo6} rings are linked together through one octahedral FeⅡ ion to generate a sandwich-type cluster with rigorous (1-) symmetry. Moreover, these clusters are further linked into a three-dimensional framework by hydrogen bonds.