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Cook, Brian J.; Di Francesco, Gianna N.; Ferreira, Ricardo B.; Lukens, James T.; Silberstein, Katharine E.; Keegan, Brenna C.; Catalano, Vincent J.; Lancaster, Kyle M.; Shearer, Jason; Murray, Leslie J.
Inorganic chemistry, 09/2018, Volume: 57, Issue: 18Journal Article
Reaction of the tricopper(I)–dinitrogen tris(β-diketiminate) cyclophane, Cu3(N2)L, with O-atom-transfer reagents or elemental Se affords the oxido-bridged tricopper complex Cu3(μ3-O)L (2) or the corresponding Cu3(μ3-Se)L (4), respectively. For 2 and 4, incorporation of the bridging chalcogen donor was supported by electrospray ionization mass spectrometry and K-edge X-ray absorption spectroscopy (XAS) data. Cu L2,3-edge X-ray absorption data quantify 49.5% Cu 3d character in the lowest unoccupied molecular orbital of 2, with Cu 3d participation decreasing to 33.0% in 4 and 40.8% in the related sulfide cluster Cu3(μ3-S)L (3). Multiedge XAS and UV/visible/near-IR spectra are employed to benchmark density functional theory calculations, which describe the copper–chalcogen interactions as highly covalent across the series of Cu3(μ-E)3+ clusters. This result highlights that the metal–ligand covalency is not reserved for more formally oxidized metal centers (i.e., CuIII + O2– vs CuII + O–) but rather is a significant contributor even at more typical ligand-field cases (i.e., Cu3 II/II/I + E2–). This bonding is reminiscent of that observed in p-block elements rather than in early-transition-metal complexes.
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