Abstract: | Potassium Tetrachlorooxomolybdate(V), KMoOCl4 KMoOCl4 was obtained at 200 °C in small yield as a side‐product from the reaction of S2Cl2 with molybdenum which contained 0.7% of potassium (the main product was MoS2Cl3). Attempts to increase the yield by adding stoichiometric amounts of KOH or of KCl + H2O failed. An attempt to produce KMoOCl4 by the reduction of MoOCl4 with KI yielded K3Mo2Cl9 and a small amount of K2MoOCl5. The crystal structure of KMoOCl4 is monoclinic, space group P21/c, a = 657,1; b = 901,6; c = 2327,3 pm; β = 92,81°, Z = 8. Square‐pyramidal MoOCl4– ions are associated to infinite zigzag chains by Mo…Cl contacts. |