Bbo multinuclear probe

All UV-vis absorption spectra of NCs dissolved in DMF were recorded using an Agilent 8453 diode array spectrometer, with the background corrected by using a DMF blank. Solid samples were dissolved in DMF to make a dilute solution, which was transferred to a 1 cm path length quartz cuvette for spectral measurements.
PL spectra were measured on an FL-4500 spectrofluorometer with the same optical density (OD) of ∼0.05. In these experiments, the NC solutions were prepared in DMF at a concentration of less than 1 mg mL^–1.
Absolute quantum yields (QYs) were measured with dilute solutions of NCs (0.05 OD absorption at 445 nm) on a HORIBA FluoroMax-4P.
³¹P NMR spectra were acquired using a Bruker 600 Avance III spectrometer equipped with a Bruker BBO multinuclear probe (BrukerBioSpin, Rheinstetten, Germany). To achieve a sufficient signal-to-noise ratio, the ³¹P NMR spectra were recorded by collecting 1k scans with a recycle delay time of 5 s.
Electrospray ionization time-of-flight mass spectrometry (ESI-TOF-MS) measurements were performed on a MicrOTOF-QIII high-resolution mass spectrometer.

All UV-vis absorption spectra of nanoclusters were recorded using an Agilent 8453 diode array spectrometer. PL spectra were measured on a FL-4500 spectrofluorometer with the same optical density of 0.1. ESI-MS measurements were performed by MicrOTOF-QIII highresolution mass spectrometer. The sample was directly infused into the chamber at 5 μL/min. For preparing the ESI samples, nanoclusters were dissolved in DMF/NMP/TMS (1 mg/mL) and diluted (v/v = 1:2) by methanol. ¹³³Cs and ³¹P NMR spectra were acquired using a Bruker 600 Avance III spectrometer equipped with a Bruker BBO multinuclear probe (BrukerBioSpin, Rheinstetten, Germany). The Ag₂₉-based assemblies were imaged with an aberration-corrected HAADF-STEM technique after the solvent that contained Ag₂₉-based assemblies was dropped casting onto ultrathin carbon film TEM grids. The microscope employed was a FEI Themis Z. The electron beam energy was 200 kV. The collecting angle HAADF detector was used to collect signals scattered between 52 (inner angle) and 200 (outer angle) mrad (camera length of 146 mm). The aberration-corrected HAADF-STEM image was obtained by Thermo Scientific Velox software using 1024^*1024 pixels and dwell time was set to 10 us.