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5 protocols using ecx 400 mhz instrument

1

Synthesis and Characterization of Gold(III) Complexes

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All commercially available reagents were used as received. The solvents used in this study were dried by standard procedures. [O(AuPPh3)3]BF4]([Au3O])27 (link) and 8-Indonaphthalen-1-amine46 (link) were prepared according to the published methods. Complexes 2 and 3 were synthesized according to our previous work14 (link). 1H-, 13C-, 31P-NMR and H-H COSY were carried out on a JEOL ECX-400 MHz instrument. H-C HMBC were carried out on a Bruker Avance 600 MHz instrument. The UV light irradiation experiment was carried out using Agilent Cary Series UV-vis-NIR. High-resolution mass spectra were obtained on a Thermo Scientific Exactive Orbitrap instrument with an ESI mode. Stopped-flow measurements were carried out using Applied Photophysics Chirascan SX20 Stopped-Flow Spectrometer. 1H-, 13C-, 31P-NMR, H-H COSY, H-C HMBC and high-resolution mass spectra are shown in Supplementary Figs. 1935.
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2

Characterization of Chemical Compounds

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All commercially available chemicals were used without further purification. The solvents used in this study were processed by standard procedures. 1H-NMR experiments were carried out on a JEOL ECX-400 MHz instrument. DOSY experiment was carried out on a Bruker Avance 600 MHz instrument using a 5 mm TXI H-C/N-D Z-GRD probe. 2D sequence for diffusion measurements were conducted using stimulated echo with 1 spoil gradient. Mass spectra were obtained using a Thermo Scientific Exactive Orbitrap instrument. UV-vis measurements were performed using Agilent Cary Series UV-Vis-NIR. EPR experiments were carried out using JEOL JES-FA200 ESR Spectrometer and Bruker E580. Elemental analyses were recorded on a Thermo FlashEA 1112 elemental analyzer. The details of X-ray crystallographic measurements are summarized in Supplementary Data 5 and 6.
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Synthesis and Characterization of Py[7] Nanoparticles

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All commercially available chemicals were used without further purification. Heptmethylazacalix[7]pyridine (Py[7]) was synthesized according to a literature method by a [3 + 4] fragment coupling protocol between a terminal dibrominated linear trimer and a terminal diaminated linear tetramer.20 (link) The solvents used in this study were processed by standard procedures. 1H NMR experiments were carried out on a JEOL ECX-400 MHz instrument. The morphology and size distribution of the as-prepared 1- to 3-NP nanoparticles were determined with a Hitachi H-7650 transmission electron microscope. X-ray photoelectron spectroscopy was performed on a Thermo Scientific ESCALab 250Xi using 200 W monochromated Al Kα radiation. The 500 μm X-ray spot was used for XPS analysis. The base pressure in the analysis chamber was about 3 × 10–10 mbar. Typically the hydrocarbon C 1s line at 284.8 eV from the adventitious carbon was used for energy referencing.
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Synthesis of Octamethylazacalix[8]pyridine

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All commercially available chemicals were used without further purification. Octamethylazacalix[8]pyridine (Py[8]) was synthesized according to the literature method by the [3 + 5] fragment coupling protocol between a terminal dibrominated linear trimer and a terminal diaminated linear pentamer.25 (link) The solvents used in this study were processed by standard procedures. 1H and 13C NMR experiments were carried out on a JEOL ECX-400 MHz instrument. Elemental analyses were recorded on a Thermo FlashEA 1112 elemental analyzer. Mass spectra were obtained using a Thermo Scientific Exactive Orbitrap instrument. Infrared spectra were recorded on a Perkin-Elmer spectrum 100 FT-IR spectrometer.
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5

Characterization of Gold Complexes

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All commercially available chemicals were used without further purification. The solvents used in this study were dried by standard procedures. All reactions were carried out under a nitrogen atmosphere unless otherwise noted. [O(AuPPh3)3](BF4),18 2-(R,R)14 (link) and 3-(R,R)14 (link) were prepared according to the published methods. 1H and 31P NMR experiments were carried out on a JEOL ECX-400 MHz instrument. The samples were heated to the target temperature for 10 min and 1H and 31P NMR experiments were carried out in situ. CD and UV-vis measurements were carried out on a Jasco J-815 circular dichroism spectropolarimeter, using 1 cm cuvettes and with pre-dried dimethyl sulfoxide as solvent. The samples were heated to the target temperature for 10 min and the CD and UV-vis spectra were monitored in situ. For the CD measurements, two accumulations of standard sensitivity at a scan rate of 100 nm min–1 and data pitch of 0.5 nm were averaged. Anisotropy factors were calculated according to g = θ [mdeg]/(32 980 × A) using the UV-vis spectrum data measured by the CD spectrometer. For time-course measurements, the change of temperature begins to detect the change of the CD response at specific wavelengths, which was followed in 0.5 s intervals at different temperatures. Mass spectra were obtained using a Thermo Scientific Exactive Orbitrap instrument.
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