Abstract: A new hybrid organic–inorganic compound [Cd(en)3]MoO4 was prepared from the hydrothermal reaction of (NH4)6Mo7O24·4H2O, CdCl2·2.5H2O, H2C2O4, ethylenediamine and H2O at 120°C. The compound crystallizes in the trigonal system, space group with a=16.2087(14)Å, c=9.8816(17)Å, V=2248.3(5)Å3, Z=6 and R1=0.0240 for 1627 observed reflections. Single crystal X-ray diffraction revealed that the structure is composed of MoO4 2− anions and [Cd(en)3]2+ complex cations, which are held together into a three-dimensional network via hydrogen-bonding interactions. The [Cd(en)3]2+ cations in the crystal structure exhibit two configurations, Λ(δδδ) and Δ(λλλ), as a pair of enantiomers due to the D 3d symmetry. Other characterizations by elemental analysis, IR and thermal analysis are also described. [Copyright &y& Elsevier]