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Table 1: Relevant 1H NMR signals in DMSO-d6 (300 MHz, δ ppm, internal TMS) of
the free ligand 1, the corresponding complexes 2,-4 and Δ (=δcomplex–δligand) values. ss=sharp singlet; wb=weak broad. a vide Figure 1 for the proton numbering system. b CH3OH signals of these complxes appear at δ 13.65 (-OH) and δ 3.40 (CH3-) respectively. c Due to low solubility of 4, neither the multiplicity of the CH(1´) signal could be characterized nor the NH(8) signal could be located. d Structural formulas of the ancillary ligand anions, dedtc´ and aet2- along with the proton numbering system of the latter, are shown in Scheme 1.The 2D NMR spectral data of the corresponding free ligands are included in the supplementary materials (Figures S–1 and S–2). e The phenyl ring proton signals of the Ph4P(+) countercation of 4, appear at δ 8.20 (2H, quartet) and δ 7.83 (3H, complex multiplet); the corresponding signals of Ph4PBr appear at δ 7.97 and δ 7.78 respectively. |