Thermal or chemical treatment of crystalline 4,4′‐bipyridinium salts of [MCl4]2− (M=Co, Zn, Fe, or Pt) leads to HCl loss and formation of coordination network solids [{MCl2(4,4′‐bipy)}n]. For M=Co, Zn, and Fe, these solids can also be prepared by mechanochemical means. Their exposure to HCl vapor or the mechanochemical reaction of metal dichlorides with [4,4′‐H2bipy]Cl2 gives [4,4′‐H2bipy]2+ salts of [CoCl4]2−, [ZnCl4]2−, and, for the first time, [FeCl4]2−.
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