Loop shaped dicarboxylate-bridged dimolybdenum(II) bisphosphine compounds--a rational synthesis

Dalton Trans. 2014 Nov 7;43(41):15367-74. doi: 10.1039/c4dt01560f.

Abstract

The reaction of the tetrametallic molecular loop [(CH3CN)6Mo2(OOC-C4H6-COO)]2[BF4]4 (1) (1 equiv.) with 2 equiv. of bis(diphenylphosphino)amine (dppa), 1,2-bis(diphenylphosphino)ethane (dppe) and bis(diphenylphosphino)methane (dppm) in propionitrile leads to the formation of the still tetrametallic complexes [(CH3CH2CN)4(X)Mo2(OOC-C4H6-COO)]2[BF4]4 (X = dppa (2), dppe (3), dppm (4)), also displaying a loop structure. All three complexes are characterized by NMR spectroscopy ((1)H, (11)B, (13)C{(1)H}, (19)F, (31)P{(1)H}), IR spectroscopy, elemental analysis, TG-MS measurements and UV-vis spectroscopy, compounds 2 and 3 additionally by X-ray single crystal diffraction.