| Solubility | Quite soluble in CHCl₃, acetone and THF |
|---|---|
| ¹H NMR (CDCl₃) | Sharp resonances were observed |
| ¹H NMR (400 MHz, chloroform-d, 21 °C) | δ 0.90 (t, 3H), 1.40 (q, 2H), 2.95 (s, 6H) |
| ¹³C{¹H} NMR (100.6 MHz, chloroform-d, 21 °C) | δ 8.14, 31.24, 31.59, 37.35 |
| Di-ATR-FTIR (cm⁻¹) | 2955, 2909, 2844 (νC−H); As−S stretches are below 400 cm⁻¹ |
| Elemental analysis | Calc. for C₆H₁₁AsS₃: C, 28.34; H, 4.36; Found: C, 28.70; H, 4.21 |
| DLS (0.250 mM in chloroform, before sonication) | Particle sizes < 5 nm in diameter |
| DLS (0.250 mM in chloroform, after sonication) | Broad particle-size distribution ranging from 50–400 nm |
| DLS (0.250 mM, 20 °C, before sonication) | No signal in hexanes; particles < 5 nm in diameter in acetone; particles between 20 and 120 nm in THF |
| DLS (0.250 mM, 20 °C, after 5 min sonication at 20 kHz and 40 % amplitude) | Particle sizes greater than 50 nm in hexanes, chloroform, acetone and THF; particle-size distributions were broad and somewhat inconsistent from run to run |
| TEM (0.250 mM in acetone or chloroform, 60 keV) | Circular hollow structures |
| Fluorescence spectroscopy (502 nm excitation, Nile Red in acetone, after water addition) | Presence of the excitation source attributed to scattering off of particles |
| ¹H and ¹³C NMR and Di-ATR-FTIR spectra | Image data were not transcribed |
| DLS graphs, TEM images and fluorescence spectrum | Image data were not transcribed |
Olivia H. Villanueva, Lina M. Delgado, Lauren A. Moran, Mychele Jorns, Dimitri Pappas, Anthony F. Cozzolino. “Pnictogen-bond-directed self-assembly of Sb and As cages enables partitioning of organic reaction media.” ChemRxiv (). https://doi.org/10.26434/chemrxiv.15004988/v3
| Solubility | Insoluble in CHCl₃, acetone, THF and hexanes; solubility in DMSO was observed |
|---|---|
| ¹H NMR | Signals could only be observed in d₆-DMSO |
| DLS (0.250 mM, 20 °C, after 5 min sonication at 20 kHz and 40 % amplitude) | Very reproducible particle-size distributions of 200–600 nm in THF, acetone and chloroform; broader distributions in hexanes |
| Fluorescence spectroscopy (502 nm excitation, Nile Red in acetone, before and after water addition) | Presence of the excitation source due to scattering off of particles |
| DLS graphs, TEM images and fluorescence spectrum | Image data were not transcribed |
| Identifier | 2 |
|---|---|
| DLS (0.250 mM in chloroform, after sonication) | Broad particle-size distribution from 8–200 nm |
| DLS (0.250 mM in acetone, chloroform, hexanes or THF, after 5 min sonication at 20 kHz and 40 % amplitude) | Broad, inconsistent particle-size distribution from run to run, ranging from 3–600 nm across all tested solvents |
| DLS graphs | Image data were not transcribed |
| DLS acquisition (0.250 mM in acetone, chloroform, hexanes or THF, 20 °C; after 5 min sonication at 20 kHz and 40 % amplitude) | Samples prepared in triplicate; 120 s equilibration followed by three 30 s scans |
|---|---|
| TEM (0.250 mM in hexanes or THF, 60 keV) | No apparent vesicles were visible; debris of the arsenic cages or previously formed vesicles remained on the grid |
| Intensity-weighted DLS, reporting qualifier | Inherently biased toward larger particles and therefore does not accurately represent the relative particle-number distribution |
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