[{Cu3WS3Cl}(PPh3)3O], Directed Synthesis of a Compound Containing Different Metal Atoms in a Cu-bane-like Skeleton
✍ Scribed by Prof. Dr. Achim Müller; Dr. Theng Khing Hwang; Dipl.-Chem. Hartmut Bögge
- Publisher
- John Wiley and Sons
- Year
- 1979
- Tongue
- English
- Weight
- 212 KB
- Volume
- 18
- Category
- Article
- ISSN
- 0044-8249
No coin nor oath required. For personal study only.
✦ Synopsis
iron, and ruthenium containing bridging p2-CS groups have recently also been described"'. To our knowledge, (5) is the first complex in which carbon monosulfide links three metal atoms together, and thus represents an example of the hitherto missing last member of the series L,M CS, L,,M,(k,-CS), L,,M3(p3-CS) established over 20 years ago in the case of the CO ligand.
Table 1. Spectroscopic data of complexes ( 5)-(X) (5): 'H-NMR ([D,,]-benzene): 6=4.50 (s). IR (KBr): 1075 (s), 1039 (s) cm ' (region expected for wi-C S stretching vibrations). MS: m / e = 4 4 8 ( M ' with correct isotopic satellites). (6): 'H-NMR ([D1]-nitromethane): 8 = 5 . l l (15H: 5 ) . 3.89 (3H; s). IR (KBr): 1008 (s), 997 (s) cm (7); 'H-NMR (ID,]-nitromethane): 6 = 5 . l 6 (15H; s). 4.45 (2H: q. J H H = 7 H7). 1.95 (3H; I, J H H = ~ Hz). (8); 'H-NMR ([D6]-acetone): 6=4.95 (s). IR (THF): u(CO)=2050, 1970 (sh), '. 1925, 1895 cm I .
Experimental
A solution of (1) (330 mg, 1.2 mmol) and (4) (1 g, 2.4 mmol) in benzene (15 ml) is heated under gentle reflux for 5 h. A first crop of (5) crystallizes on cooling. The solvent is stripped off completely under vacuum, the residue washed several times with hexane, and recrystallized from THF/hexane. (51, black crystals, dec. pt. = 289 "C; yield 450 mg.