The folder contains the data for each spectrum reported in the figures of the manuscript and the Supporting Information. Main manuscript: The files for Figure 5 contains data of: (1) XRD shown in iteration 1-2 (2) XRD shown in iteration 3 (3) XRD shown in iteration 4 (4) XRD shown in iteration 5 (5) XRD shown in iteration 6 (6) XRD shown in iteration 7-8 (7) XRD shown in iteration 9 The files for Figure 6 contains data of: (1) XRD of RD Cu NCs (Figure 6e) (2) 31P{1H} NMR of a solution containing CuI and TOP in OLAM (green in Figure 6g) (3) 31P{1H} NMR of the TOP reference (purple in Figure 6g) Supporting Information: The files for Figure S2 contains data of: (1) 31P{1H} NMR of a solution containing CuBr and TOP in OLAM (Figure S2A) (2) For the 31P{1H} NMR of the TOP reference (Figure S2A), see the file in Figure 6g (3) 31P{1H} NMR of a solution containing CuBr and TMP in OLAM (Figure S2B) (4) 31P{1H} NMR of the TMP reference (Figure S2B) The file for Figure S5 contains data of: (1) 31P{1H} NMR of a solution containing CuCl, CuBr, TOP and TMP in OLAM (Figure S5) (2) For the 31P{1H} NMR of the TOP reference, see the file in Figure 6g (3) For the 31P{1H} NMR of the TMP reference, see the file in Figure S2 The file for Figure S6 contains data of: (1) For the XRD, see the file in Figure 5 for iteration 3 The file for Figure S7 contains data of: (1) For the XRD, see the file in Figure 5 for iteration 6 The file for Figure S10 contains data of: (1) The size statistics of the Cu RD NCs (Figure S10) The files for Figure S11 contains data of: (1) For the XRD of the Cu RDs NCs, see the file in Figure 6e (2) XRD of Cu cubes (Figure S11B) (3) XRD of Cu octahedra (Figure S11B)