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)(μPh2P(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) Å, b = 10.403(1) Å, c = 16.987(7) Å, 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.