MoV-MoVI cationic ordering in the layered molybdate (C2H10N2)[Mo4O12]

The mixed valence Mo-V-Mo-VI layered tetramolybdate (C2H10N2)[Mo4O12] has been hydrothermally synthesized (180 degrees 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) Angstrom, beta = 117.549(1)degrees and Z = 4 at 20 degrees C. The structure was solved from single crystal X-ray diffraction data. Full matrix anisotropic least-squares techniques led to a conventional R-1(F-o) factor of 0.044 [wR(2)(F-o(2)) = 0.107] for 2885 reflections [I > 2 sigma(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.