Abstract: | An organo‐spaced molybdenum thiocomplex [ H3NCH2CH2‐NH3][Mo3S13] has been synthesized under hydrothermal condition and the structure of the compound was determined by single‐crystal X‐ray diffraction. The title compound crystallizes in the monoclinic space group C2/c with a = 1.81157 (18), b = 1.04549(9), c = 2.04892(19) nm, β= 107.184 (2)°, Z = 8 and V = 3.7074(6) nm3. The inorganic part of the compound consists of a Mo3 triangle capped by an apical μ3‐sulfur atom, with each Mo atom being also coordinated to one terminal disulfur ligand and two bridging disulfur ligands. The negative charges on the inorganic cluster are balanced by the diprotonated ethylenediamine cations [ H3NCH2CH2‐NH3]2+ located in the space between the clusters. |