The dataset contains 31 P-NMR spectra as .fid files used to characterize palladium complexes formed during the in-situ generation of Pd(0) catalysts from Pd(II) precatalysts in cross-coupling reactions. The reduction process was examined via NMR to evaluate the influence of reagents, solvents, bases, ligands, and counterions. The spectra represent the optimal results obtained from the screening of each parameter
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