The synthesis and characterization of a homologous series of T-shaped {MNO} nitrosyl complexes of the form [M(PR)(NO)] (M = Pd, Pt; R = Bu, Ad) are reported. These diamagnetic nitrosyls are obtained from monovalent or zerovalent precursors by treatment with NO and NO, respectively, and are notable for distinctly bent M-NO angles of ∼123° in the solid state. Adoption of this coordination mode in solution is also supported by the analysis of isotopically enriched samples by N NMR spectroscopy. Effective oxidation states of M/NO are calculated, and metal-nitrosyl bonding has been interrogated using DFT-based energy decomposition analysis techniques. While a linear nitrosyl coordination mode was found to be electronically preferred, the M-NO and P-M-P angles are inversely correlated to the extent that binding in this manner is prevented by steric repulsion between the bulky ancillary phosphine ligands.
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| http://dx.doi.org/10.1021/acs.inorgchem.3c03434 | DOI Listing |
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