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Preparation and Characterization of Bis[(μ-acetato)halo(μ-bis(diphenylphosphino)amine)molybdenum(II)] Complexes

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posted on 31.07.1996, 00:00 by Deirdre I. Arnold, F. Albert Cotton, Fritz E. Kühn
Molecules of the formula Mo2X2(OAc)2(μ-dppa)2 (X = Cl (2), Br (3), I (4); dppa = bis(diphenylphosphino)amine; OAc = CH3COO-) can be synthesized by the reaction of Mo2(OAc)4 (1) with dppa and (CH3)3SiX. All three compounds were characterized by IR and UV−visible spectroscopy, mass spectrometry, and 31P{1H} NMR spectroscopy. Single-crystal diffraction studies yield the following pertinent crystal data:  for 2·2EtOH, orthorhombic Pbca (No. 61), a = 16.830(2) Å, b = 20.310(4) Å, c = 16.751(2) Å,V = 5726(2) Å3, Z = 4; for 3·2(toluene), monoclinic C2/c (No. 15), a = 22.481(2) Å, b = 19.151(9) Å, c = 14.358(2) Å, β = 95.19(2)°, V = 6156(3) Å3, Z = 4; for 4·EtOH·CH3CN, monoclinic P21/c (No. 14), a = 20.607(9)Å, b = 16.020(3) Å, c = 17.189(5) Å, β = 95.81(2)°, V = 5645(3) Å3, Z = 4. The Mo−Mo distances for compounds 24 are 2.158(1), 2.176(1), and 2.164(1) Å, respectively. Both crystallographic data and physical measurements indicate that 2 and 3 have nearly identical Mo−X bond distances while those in 3 and 4 differ more significantly; the spectroscopic data bear this out. The Mo−O and Mo−P distances are very similar in all three of the complexes reported.

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