Synthesis, Crystal Structure, and Relativistic DV-Xα Calculation of a μ-Oxido-μ-molybdato(VI)-bridged Dinuclear Oxidomolybdenum(V) Complex with 2-(3-Aminopropyl)aminoethanethiol

A μ-O-μ-MoVIO4-bridged dinuclear oxidomolybdenum(V) complex with 2-(3-aminopropyl)aminoethanethiol (Hapaet), [Mo3O7(apaet)2]·2CH3OH, was prepared. The crystal structure was determined by the single-crystal X-ray diffraction method at 293 K. It crystallizes in the monoclinic space group P21/n with a = 16.558(3)Å, b = 8.9725(13)Å, c = 17.193(3)Å, β = 90.192(2)°, V = 2554.3(7)Å3, Dx = 1.899 g/cm3, and Z = 4. The R1 [I > 2σ(I)] and wR2 (all data) values are 0.0331 and 0.0768, respectively, for all 6166 independent reflections. The two molybdenum atoms are bridged by an oxido-O atom and MoO42− in a distorted octahedral geometry with oxido-O and meridional NNS-donor atoms of apaet−. A relativistic DV-Xα calculation supported the MoV2MoVI mixed-valent state.