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The preparation, characterization and electrochemical and photophysical properties of a series of desymmetrized heteroleptic [Cu(P^P)(N^N)][PF 6 ] compounds are reported. The complexes incorporate the chelating P^P ligands bis(2-(diphenylphosphanyl)phenyl)ether (POP) and (9,9-dimethyl-9 H -xanthene-4,5-diyl)bis(diphenylphosphane) (xantphos), and 6-substituted 2,2'-bipyridine (bpy) derivatives with functional groups attached by -(CH 2 )  n  - spacers: 6-(2,2'-bipyridin-6-yl)hexanoic acid ( 1 ), 6-(5-phenylpentyl)-2,2'-bipyridine ( 2 ) and 6-[2-(4-phenyl-1 H -1,2,3,triazol-1-yl)ethyl]-2,2'-bipyridine ( 3 ). [Cu(POP)( 1 )][PF 6 ], [Cu(xantphos)( 1 )][PF 6 ], [Cu(POP)( 2 )][PF 6 ], [Cu(xantphos)( 2 )][PF 6 ], and [Cu(xantphos)( 3 )][PF 6 ] have been characterized in solution using multinuclear NMR spectroscopy, and the single crystal structure of [Cu(xantphos)( 3 )][PF 6 ]  .  0.5Et 2 O was determined. The conformation of the 6-[2-(4-phenyl-1 H -1,2,3,triazol-1-yl)ethyl]-substituent in the [Cu(xantphos)( 3 )] + cation is such that the α- and β-CH 2 units reside in the xanthene 'bowl' of the xantphos ligand. The 6-substituent desymmetrizes the structure of the [Cu(P^P)(N^N)] + cation and this has consequences for the interpretation of the solution NMR spectra of the five complexes. The NOESY spectra and EXSY cross-peaks provide insight into the dynamic processes operating in the different compounds. For powdered samples, emission maxima are in the range 542-555 nm and photoluminescence quantum yields (PLQYs) lie in the range 13-28%, and a comparison of PLQYs and decay lifetimes with those of [Cu(xantphos)(6-Mebpy)][PF 6 ] indicate that the introduction of the 6-substituent is not detrimental in terms of the photophysical properties.

Desymmetrizing Heteroleptic [Cu(P^P)(N^N)][PF6] Compounds: Effects on Structural and Photophysical Properties, and Solution Dynamic Behavior