“…The surface composition was initially analyzed with 1 H NMR on Cu 3– x P particles, washed to remove excess precursors, which was indicative of long alkyl chains consistent with HDA as the primary, surface-bound ligand (Figure S18). Additionally, X-ray photoelectron spectroscopy (XPS) of the carbon (C) and nitrogen (N) 1s regions (Figure S19) is representative of HDA binding environments according to previous literature reports. ,, Of note, the Cu and P 2p binding region (Figure A and B) demonstrates the characteristic Cu 3– x P environments, ,− while the satellite Cu(II) peak (Figure B) and P–O peak at 134 eV likely corresponds to surface oxides. − , Finally, Cu 3 PSe 4 was characterized with XPS for Cu, P, Se, and C bonding environments (Figure S20). The core bonding environments (Cu, P and Se) were consistent with previous reports of Cu 3 PSe 4 and Cu 3 PS 4 , − , whereas the C region had similar peaks to Cu 3– x P NPs but a decrease in the C-NH 2 environment (Figure S20D).…”