SYNTHESIS OF A MULTIPLY-BONDED DITUNGSTEN HYDRIDE COMPLEX, W-2(MU-H) (MU-O2CC6H5)CL-4(DPPM)(2)

The use of Me(3)SiCl in the reaction of W-2(O2CC6H5)(4) with dppm resu lted in the metal-halide-bonded complex, W-2(mu-H)(mu-O2CC6H5)Cl-4(dpp m)(2). The presence of the bridging hydride was confirmed by H-1 NMR s pectra of the sample. The W-W bond distance of 2.554(2) Angstrom is in dicative of a multiple bond. If the reaction is performed with fresh M g3SiCl, the P-31 NMR spectra of the reaction mixture verifies that a s mall amount of the quadruply-bonded product, W2Cl4(dppm)(2), is produc ed. Crystallographic data for W-2(mu-H)(mu-O2CC6H5)Cl-4(dppm)(2) are a s follows: monoclinic, space group P2(1)/c with a=19.171(11), b=14.901 (8), c=24.142(12) Angstrom, beta=111.94(5)degrees, V=6397(6) Angstrom( 3), Z=4.