Syntheses, Structures and Spectroscopic Studies of Quadruply Bonded Complexes Containing Bridging Acetate and η3‐etp Ligands (etp = Ph2PCH2CH2P(Ph)CH2CH2PPh2)

The quadruply bonded complexes containing bridging acetate and polydentate phosphine ligands of the type Mo2(O2CCR3)XJ(η3-etp) (R = H, X = Br, 1; R = F, X = CI, 2; R = F, X = Br, 3; etp = Ph2PCH2CH2P(Ph)CH2CH2PPh2) were prepared by reactions of Mo2(O2CCR3)X2(PPh3)2 with etp in CH2X2. Their UV-vis and 31P{1H}-NMR spectra have been recorded, and the structure of 1 has been determined by X-ray crystallography. Crystal data for 1·2CH2Br2: space group P21/c, a = 13.924(7) A, b = 21.157(4) A, c = 14.427(5) A, β = 101.82(3)°, V = 4159(2) A3, Z = 4, with final residuals R = 0.0797 and Rw = 0.0793. The absorption wavelengths of the δ δ* transitions and the chemical shifts and the coupling constants of the 31P{1H}-NMR spectra of these complexes are dependent on the natures of the halogen atoms and the acetate ligands.