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Heteronuclear calcium–iron carbonyl cation complexes in the form of [CaFe(CO)  n  ] +  ( n =5–12) are produced in the gas phase. Infrared photodissociation spectroscopy in conjunction with quantum chemical calculations confirm that the  n =10 complex is the coordination saturated ion where a Fe(CO) 4  fragment is bonded with a Ca(CO) 6  fragment through two side‐on bridging carbonyl ligands. Bonding analysis indicates that it is best described by the bonding interactions between a [Ca(CO) 6 ] 2+  dication and an [Fe(CO) 4 ] −  anion forming a Fe→Ca d−d dative bond in the [(CO) 6 Ca–Fe(CO) 4 ] +  structure, which enriches the pool of experimentally observed complexes of calcium that mimic transition metal compounds. The molecule is the first example of a heteronuclear carbonyl complex featuring a d−d bond between calcium and a transition metal.

Highly Coordinated Heteronuclear Calcium–Iron Carbonyl Cation Complexes [CaFe(CO) n ] + ( n =5–12) with d−d Bonding