Insights into the κ-P,N Coordination of 1,3,5-Triaza-7-phosphaadamantane and Derivatives: κ-P,N-Heterometallic Complexes and a (15)N Nuclear Magnetic Resonance Survey

1,3,5-三氮杂-7-磷杂金刚烷及其衍生物的κ-P,N配位机制研究:κ-P,N-异金属配合物及<sup>15</sup>N核磁共振谱分析

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Abstract

Complexes {[(PTA)(2)CpRu-μ-CN-1κC:2κ(2)N-RuCp(PTA)(2)-ZnCl(3)]}·2DMSO (13) {[ZnCl(2)(H(2)O)]-(PTA-1κP:2κ(2)N)(PTA)CpRu-μ-CN-1κC:2κ(2)N-RuCp(PTA)(PTA-1κP:2κ(2)N)-[ZnCl(2)(H(2)O)]}Cl (14), [RuCp(HdmoPTA)(PPh(3))(PTA)](CF(3)SO(3))(2) (20), [RuCp(HdmoPTA)(HPTA)(PPh(3))](CF(3)SO(3))(3) (21), and [RuCp(dmoPTA)(PPh(3))(PTA)](CF(3)SO(3)) (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 (15)N 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). (15)N detection via (1)H-(15)N heteronuclear multiple bond correlation allowed the construction of a small library of (15)N chemical shifts that shed light on important features regarding κN-coordination in PTA and its derivatives.

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