Unexpected XPS Binding Energy Observations Further Highlighted by DFT Calculations of Ruthenocene-Containing [Ir(III)(ppy)(2)(RCOCHCORc)] Complexes: Cytotoxicity and Crystal Structure of [Ir(ppy)(2)(FcCOCHCORc)]

通过对含钌茂的[Ir(III)(ppy)(2)(RCOCHCORc)]配合物的DFT计算,进一步揭示了意外的XPS结合能观察结果:[Ir(ppy)(2)(FcCOCHCORc)]的细胞毒性和晶体结构

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Abstract

The series of iridium(III) complexes, [Ir(ppy)(2)(RCOCHCOR')], with R = CH(3) and R' = CH(3) (1), Rc (2), and Fc (3), as well as R = Rc and R' = Rc (4) or Fc (5), and R = R' = Fc (6), ppy = 2-phenylpyridinyl, Fc = Fe(II)(η(5)-C(5)H(4))(η(5)-C(5)H(5)), and Rc = Ru(II)(η(5)-C(5)H(4))(η(5)-C(5)H(5)), has been investigated by single-crystal X-ray crystallography and X-ray photoelectron spectroscopy (XPS) supplemented by DFT calculations. Here, in the range of 3.74 ≤ Σχ(R) ≤ 4.68, for Ir 4f, Ru 3d and 3p and N 1s orbitals, binding energies unexpectedly decreased with increasing Σχ(R) (Σχ(R) = the sum of Gordy group electronegativities of the R groups on β-diketonato ligands = a measure of electron density on atoms), while in Fe 2p orbitals, XPS binding energy, as expected, increased with increasing Σχ(R). Which trend direction prevails is a function of main quantum level, n = 1, 2, 3…, sub-quantum level (s, p, d, and f), initial state energies, and final state relaxation energies, and it may differ from compound series to compound series. Relations between DFT-calculated orbital energies and Σχ(R) followed opposite trend directions than binding energy/Σχ(R) trends. X-ray-induced decomposition of compounds was observed. The results confirmed good communication between molecular fragments. Lower binding energies of both the Ir 4f(7/2) and N 1s photoelectron lines are associated with shorter Ir-N bond lengths. Cytotoxic tests showed that 1 (IC(50) = 25.1 μM) and 3 (IC(50) = 37.8 μM) are less cytotoxic against HeLa cells than cisplatin (IC(50) = 1.1 μM), but more cytotoxic than the free β-diketone FcCOCH(2)COCH(3) (IC(50) = 66.6 μM).

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