A series of representative late d-block metal complexes bearing a rigid bis(phosphine) ligand, iPrP-Ace-PPh (L, Ace = acenaphthene-5,6-diyl), was prepared and fully characterized by various techniques, including multinuclear NMR and single-crystal X-ray diffraction. The heteroleptic nature of the peri-substituted ligand L allows for the direct observation of the J couplings in the P{H} NMR spectra. Magnitudes of J are correlated with the identity and geometry of the metal and the distortions of the ligand L.
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