Synapt g2 tandem mass spectrometer

All reagents were commercially available and used as supplied without further purification. Deuterated solvents were purchased from Cambridge Isotope Laboratory (Andover, MA). Compounds 5,^{51 (link)}6,^{51 (link)}7−10^{51 (link),66 (link)} were prepared according to modified literature procedures. NMR spectra were recorded at room temperature. 1H chemical shifts are reported relative to the residual solvent signals, and ³¹P{¹H} NMR chemical shifts are referenced to an external unlocked sample of 85% H₃PO₄ (δ = 0.0). Mass spectra were recorded on a Waters synapt G2 tandem mass spectrometer using electrospray ionization with a MassLynx operating system. Ultraviolet−visible experiments were conducted on a Hitachi U-4100 absorption spectrophotometer. Fluorescence experiments were conducted on a Hitachi F-7000 fluorescence spectrophotometer. Transmission electron microscopy investigations were performed on a JEM-2100EX instrument. For TEM, dispersions of the assemblies were dried onto carbon-coated copper support grids. A Zeiss Supra55 field-emission scanning electron microscope was used to investigate the assemblies. For scanning electron microscopy, dispersions of the assemblies were dried onto silicon wafers. High-resolution TEM and elemental mapping images were obtained using a Tecnai G2 F30 S-TWIN instrument.

All reagents were purchased from Sigma-Aldrich, Matrix Scientific, Alfa Aesar and used without further purification. Column chromatography was conducted using basic Al₂O₃ (Brockman I, activity, 58 Å) or SiO₂ (VWR, 40–60 μm, 60 Å) and the separated products were visualized by UV light or detected by ESI-TOF. NMR spectra data were recorded on a 500-MHz and 600 MHz Bruker Avance NMR spectrometer in CDCl₃, CD₃CN, CD₃OD. ESI-MS and TWIM-MS were recorded with a Waters Synapt G2 tandem mass spectrometer, using solutions of 0.01 mg sample in 1 mL of CHCl₃/CH₃OH (1 : 3, v/v) for ligands or 0.5 mg sample in 1 mL of MeCN/MeOH (3 : 1, v/v) for complexes. MALDI-TOF was carried out on Bruker AutoFlex TOF/TOF mass spectrometer.