GC analysis was performed with a flame ionisation detector using a 0.22 mm × 25 m capillary column (BP-5). The
1H and
13C NMR spectra were recorded at 400 and 100 MHz, respectively. The
1H and
13C NMR chemical shifts are reported in ppm with respect to the residual chloroform (
1H 7.26 ppm,
13C 77 ppm). The products were characterised by
1H NMR,
13C NMR, and GC-MS. The TEM and STEM images were obtained with a JEOL
JEM-ARM200F instrument at an accelerating voltage of 200 kV. Size distributions of nanoparticles were measured by counting 100 nanoparticles. ICP-AES was performed with a Shimadzu
ICPS-8100 spectrometer. XPS analysis was performed with a ULVAC-PHI
PHI5000 VersaProbe with Al Kα radiation. The measured spectra were calibrated by the C 1 s electron peak (284.5 eV). TG analysis was performed with a Thermo Plus EVO device (Rigaku, Japan) at a heating rate of 10 °C min
−1 under nitrogen flow.
All of the synthesised compounds (3a,
23a (link)3b,
23a 3c,
23a 3d,
23b 3e,
23a 3f,
23b 3g,
23e 3h,
23c 3i,
23d 5a,
24a (link)5b,
24c 5c,
24c 5d, 5e,
24b 5f,
24d and 5g
24b ) are known compounds and have been previously reported.
All of the starting materials were commercially available and used without further purification. The DMF-protected Pd NCs were prepared according to a previously reported method.
15a
Nagata T., Inoue T., Lin X., Ishimoto S., Nakamichi S., Oka H., Kondo R., Suzuki T, & Obora Y. (2019). Dimethylformamide-stabilised palladium nanoclusters catalysed coupling reactions of aryl halides with hydrosilanes/disilanes. RSC Advances, 9(30), 17425-17431.