SYNTHESIS OF COINAGE METAL CATION ADDUCTS OF NB(C(5)H(4)SIME(3))(2)H(CO) - X-RAY CRYSTAL-STRUCTURE OF [(NB(C(5)H(4)SIME(3))(2)(CO))2(MU-H)(2)CU]PF6

The reactions of Nb(C(5)H(4)SiMe(3))(2)H(CO) (2) with [Cu(MeCN)(4)]BF4, CuPPh(3)Cl/TlPF6, AgBF4, AgPPh(3)Cl/TlPF6, and Au(THT)Cl/TlPF6 lead to the new adducts [{Nb(C(5)H(4)SiMe(3))(2)(CO)}(2) .(mu-H)(2)M](+) (M = Cu (3), Ag (4, 5), Au (6)), in which the coinage metal cation is only linked to the hydride of each niobium center, whereas the reaction with [Au(PPh(3))](+) leads to [{Nb(C(5)H(4)SiMe(3))(2)(Co)}(mu-H)Au(PPh(3))]PF6 (7) The crystal structure of 3 has been determined by X-ray diffraction methods. The crystals are monoclinic, space group P2(1)/c, with Z = 4 in a unit cell of dimensions a = 13.048(5) Angstrom, b = 12.490(4) Angstrom, c = 30.131(9) Angstrom, beta = 94.52(2)degrees. The structure has been solved from diffractometer data by Patterson and Fourier methods and refined by blocked full-matrix least squares on the basis of 3001 observed reflections to R and R(w) values of 0.0460 and 0.0608, respectively.