MoV–MoVIcationic ordering in the layered molybdate (C2H10N2)[Mo4O12]

Abstract

The mixed valence Mo^V–Mo^VI layered tetramolybdate (C₂H₁₀N₂)[Mo₄O₁₂ ] has been hydrothermally synthesized (180 °C, 3 weeks, autogenous pressure). It crystallizes in the monoclinic system (space group C2) with a=11.4090(2),b=11.8227(2), c=10.2305(1) Å, β=117.549(1)° and Z=4 at 20 °C. The structure was solved from single crystal X-ray diffraction data. Full matrix anisotropic least-squares techniques led to a conventional R₁(F_o) factor of 0.044 [wR₂(F_o²)=0.107] for 2885 reflections [I>2sigma;(I)]. Its structure consists of [Mo₄O₁₂ ]^2– layers perpendicular to the c* axis, made up of an ordered organization of isolated tetrameric Mo^V clusters linked by edges to tetrameric Mo^VI ones. Ethylenediamine cations are located between the inorganic layers and ensure the connectivity of the structure via hydrogen bonds.