Reaction of Ru3(η3-NPh)(CO)10 with DPPM (diphenylphosphinomethane) has given the substituted imido complex Ru3(η3-NPh)(η-DPPM)(CO)8, the structure of which has been determined by X-ray diffraction. The compound crystallizes in the monoclinic space group P21/n with a 14.027(7), b 14.887(7), c 18.499(9) Å, β 93.52(4)° and Z = 4; R = 0.022 and Rw = 0.028 for 5006 independent reflections with I > 3 σ(I). The interaction of the imido complex with CO has been investigated under various conditions. It proved to be very robust, giving small amounts of PhNCO (or PhNHCO2Me in the presence of methanol) and Ru3(η-DPPM)(CO)10 only at 170° C and 60 atm of carbon monoxide.
SYNTHESIS AND CRYSTAL-STRUCTURE OF RU3(MU-3-NPH)(MU-DPPM)(CO)8 / M. PIZZOTTI, F. PORTA, S. CENINI, F. DEMARTIN. - In: JOURNAL OF ORGANOMETALLIC CHEMISTRY. - ISSN 0022-328X. - 356:1(1988), pp. 105-111. [10.1016/0022-328X(88)80678-8]
SYNTHESIS AND CRYSTAL-STRUCTURE OF RU3(MU-3-NPH)(MU-DPPM)(CO)8
M. Pizzotti;F. Porta;S. Cenini;F. Demartin
1988
Abstract
Reaction of Ru3(η3-NPh)(CO)10 with DPPM (diphenylphosphinomethane) has given the substituted imido complex Ru3(η3-NPh)(η-DPPM)(CO)8, the structure of which has been determined by X-ray diffraction. The compound crystallizes in the monoclinic space group P21/n with a 14.027(7), b 14.887(7), c 18.499(9) Å, β 93.52(4)° and Z = 4; R = 0.022 and Rw = 0.028 for 5006 independent reflections with I > 3 σ(I). The interaction of the imido complex with CO has been investigated under various conditions. It proved to be very robust, giving small amounts of PhNCO (or PhNHCO2Me in the presence of methanol) and Ru3(η-DPPM)(CO)10 only at 170° C and 60 atm of carbon monoxide.
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