DMF (20 mL). To the solution thus obtained was added dropwise over 10 min sulfur monochloride (0.040 mL, 0.50 mmol) in dry DMF (5.0 mL) under nitrogen at ±50 C. While being stirred overnight the reaction mixture was allowed to reach room temperature, and the resultant brown precipitate was filtered and washed with methanol. The crude product was purified by column chromatography (silica gel, carbon disulfide) and recrystallized from carbon disulfide/hexane (1:2, v/v) to afford 64.0 mg (0.141 mmol) of airstable black plate-like crystals in 27 % yield. mp (decomp.) 183.0±183.6 C. IR (KBr) [cm ±1 ] n = 2921, 2853, 1508, 1456, 959, 915, 768, 511, 468. 1 H NMR (CS 2 /CDCl 3 ) (5:1, v/v) [ppm] d = 3.29 (m, 4H). Anal. Calcd. for C 8 H 4 S 11 : C 21.25, H 0.92, S 78.19; found, C 21.22, H 0.89, S 77.89.Crystallographic Data Collection and Structure Determination: X-ray crystal structure analyses were performed for 4 and its ClO 4 ± salt. Their crystal and experimental data are shown in Table 1. Data collection and refinement conditions: Rigaku AFC-5R diffractometer, 296 K, o±2y mode up to 2y = 60, o scan speed 8.0 deg min ±1 , graphite monochromated Mo Ka radiation (l = 0.71069 ). No decay correction was applied. The structure was solved by a direct method (SHELXS86) [12]. The atomic scattering factors were taken from the International Tables for X-ray Crystallography [13]. Full-matrix least-squares refinements with all non-hydrogen atoms anisotropic were carried out for 4 and 4×ClO 4 ×(chlorobenzene) 0.5 except for the solvent molecule of the perchlorate salt, which was refined isotropically. Hydrogen atoms were included, but their positions were not refined.The potential application of monodisperse metals and semiconductor colloids in such fields as nonlinear optics, photovoltaic cells, catalysis and new laser technologies has led to research into the preparation and stabilization of nanosized particles. [1±8] The classical routes comprise
