Inorganic Chemistry, Vol.41, No.5, 1136-1139, 2002
Preparation and properties of the aqua ions [W4S4(H2O)(12)](n+) (n=5, 6) and crystal structure of (Me2NH2)(6)[W4S4(NCS)(12)]center dot 0.5H(2)O
The [3 + 1] reaction of [W3S4(H2O)(9)](4+) with [W(CO)(6)] in 2 M HCl under hydrothermal conditions (130 degreesC) gives the [W4S4(H2O)(12)](6+) cuboidal cluster, reduction potential 35 mV vs NHE (6+/5+ couple). The reduced form is obtained by controlled potential electrolysis. X-ray crystal structure was determined for (Me2NH2)(6)[W4S4(NCS)(12)].0.5H(2)O, The W-W and W-S bond lengths are 2.840 and 2.379 Angstrom, respectively.