Solvo-Thermal Application for the Synthesis of [Et4N][(μ-H)Mo2(CO)10] and its Bidentate Phosphine Derivatives and the X-ray Structure of (μ-Ph2P(CH2)2PPh2) [Mo (CO)4(NCCH3)]2

The compounds [et4n][(μ-h)(μ-ph2p(ch2)npph2)mo2(co)8] (n = 1 and 2) and their parent compound [et4n][(μ-h)mo2(co)10] were synthesized using solvo-thermal method. the ir spectra are identical with those prepared by conventional methods. protonation of [et4n][(μ-h)(μ-ph2p(ch2)npph2)mo2(co)8] using cf3co2h at -70 ° in ch3cn led to the capture of the intermediate [(co)4modppemo(co)4], which was isolated as a solid material and identified by elemental analysis, ft-ir and x-ray structure as (μ-ph2p(ch2)2pph2)[mo(co)4(ncch3)]2. the x-ray analysis show the following parameters, p2/n (no. 14), z=2, a = 11.957 (2) a, b = 10.403(1) a, c = 16.987(7) a, α = 90°, β = 108.4(2) ° , γ = 90° the structure shows a center of inversion at the middle of the hydrocarbon chain which connects the two phosphorus donor sites.