The folder contains the data for each spectrum reported in the figures of the manuscript.

The files for Figure 1 contains the data of:
(1) The size statistics of twinned Cu NCs obtained at 130°C after 2h, 20h, 70h and 120h shown in Figure 1U.

The files for Figure 2 contains data of:
(1) 31P{1H} NMR spectroscopy of DPP and of the complex shown in Figure 2A.
(2) 1H NMR spectroscopy of DPP and of the complex shown in Figure 2B.
(3) Experimetnal EXAFS data of the {CuBr(DPP)2}2 complex and the corresponding fitting shown in Figure 2C.

The files for Figure 3 contains data of:
(1) The normalized XANES spectra acquired during the reaction at 270°C used to plot the color map shown in Figure 3A.
(2) The normalized concentration of {CuBr(DPP)2}2, Cu(I/II) and Cu(0) obtained after PCA and MCR-ALS shown in Figure 3B.

The files for Figure 4 contains data of:
(1) The EXAFS data acquired at the end of the reaction at 270°C, 200°C, 150°C and 110°C with Cu foils and {CuBr(DPP)2}2 reference shown in Figure 4A.
(2) The XRD spectra acquired during the reaction at 270°C shown in Figure 4B.
(3) The XRD spectra acquired during the reaction at 150°C shown in Figure 4C.
(4) The average Cu formation rate determined by ICP-OES and the XRD normalized (111) intensity shwon in Figure 4D.