The reaction of (thf)Fe[N(SiMe3)2]2Cl with (2‐pyridylmethyl)(diphenylphosphanyl)amine (1) in hot tetrahydrofuran (THF) yields dinuclear [(ClFe)2{μ‐N(SiMe3)2}{Ph2P(NCH2Py)2}] (2) and [ClFe{Ph2P(O)‐NCH2Py}]2 (3) with the oxygen atom stemming from THF degradation. The formation of 2 requires a P–N bond cleavage and reformation leading to the tetradendate diphenyl‐bis(2‐pyridylmethylamido)phosphonium ion. If this reaction of (thf)Fe[N(SiMe3)2]2Cl with 1 is performed at room temperature, no P–N bond cleavage is observed. Instead of that, ether degradation occurs yielding [Fe4(μ4‐O)(μ2‐Cl)2(Ph2P‐NCH2Py)4] (4) with a central oxygen‐centered iron tetrahedron as well as complex 3. Recrystallization of 3 from dichloromethane leads to addition of HCl and to the formation of [FeCl2·{Ph2P(O)‐N(H)‐CH2Py}] (5). The phosphonium ion of 2 is isoelectronic to the corresponding diphenyl‐bis(2‐pyridylmethylamino)silane (6). Lithiation of 6 followed by a metathetical reaction with (thf)2FeCl2 yields the trinuclear complex [Fe3Cl2{Ph2Si(NCH2Py)2}2] (7) with antiferromagnetic interactions.
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