New efficient synthesis of the triangular cluster [W3Se4(H2O)9]4+ and X-ray structure of the first mixed-metal seleno-bridged cubane-type tungsten-tin cluster (Me2NH2)6[(SCN)9W3Se4SnCl3]·0.5H2O
摘要:
The trinuclear incomplete cuboidal [W3Se4(H2O)(9)](4+) cluster has been prepared by reacting polymeric solid W3Se7Br4 with H3PO2 in aqueous HCl solution with yields up to 50%. The mixed-metal cluster compound (Me2NH2)(6)[(SCN)(9)W3Se4SnCl3]. 0.5H(2)O (1) has been prepared by reacting [W3Se4(H2O)(9)](4+) in aqueous HCl solution with SnCl2 . 2H(2)O in the presence of Me2NH2Cl and NaSCN. Crystals of 1 are monoclinic space group C2/c, a = 42.868(6), b = 12.035(1), c = 21.976(5) Angstrom, beta = 95.69(1)degrees and Z = 8. The structure was refined by full-matrix least-squares techniques to R(Rw) = 0.0343(0.0478), The title compound 1 is the first mixed-metal seleno-bridged cubane-type tungsten-tin cluster as derivative of [W3Se4(H2O)(9)](4+). (C) 1998 Elsevier Science S.A.