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Insights into the κ‑P,N Coordination of 1,3,5-Triaza-7-phosphaadamantane and Derivatives: κ‑P,N-Heterometallic Complexes and a 15N Nuclear Magnetic Resonance Survey
Complexes {[(PTA)2CpRu-μ-CN-1κC:2κ 2 N-RuCp(PTA)2-ZnCl3]}·2DMSO (13) {[ZnCl2(H2O)]-(PTA-1κP:2κ2 N)(PTA)CpRu-μ-CN-1κC:2κ2 N-RuCp(PTA)(PTA-1κP:2κ2 N)-[ZnCl2(H2O)]}Cl (14), [RuCp(HdmoPTA)(PPh3)(PTA)](CF3SO3)2 (20), [RuCp(HdmoPTA)(HPTA)(PPh3)](CF3SO3)3 (21), and [RuCp(dmoPTA)(PPh3)(PTA)](CF3SO3) (22) were obtained and characterized, and their crystal structure together with that of the previously published complex 18 is reported. The behavior of the 1,3,5-triaza-7-phosphatricyclo[3.3.1.13,7]decane (PTA) and 3,7-dimethyl-1,3,7-triaza-5-phosphabicyclo[3.3.1]nonane (dmoPTA) ligands against protonation and κN-coordination is discussed, on the basis of 15N nuclear magnetic resonance data collected on 22 different compounds, including PTA (1), HdmoPTA (7H), and some common derivatives as free ligands (2–6 and 8), along with mono- and polymetallic complexes containing PTA and/or HdmoPTA (9–22). 15N detection via 1H–15N heteronuclear multiple bond correlation allowed the construction of a small library of 15N chemical shifts that shed light on important features regarding κN-coordination in PTA and its derivatives.