Abstract
A triangular V 38 7 2+ complex (Et 4N)[V 3S 7(Me 2dtc) 3]·CH 3CN has been obtained from a complicated reaction system containing (NH 4) 3VS 4 as a starting material. The complex crystallizes in the triclinic, space group P1̄ with crystal data: a=13.027(2), b=13.180(5), c=12.554(4) Å, a=97.00(3), β=116.21(2), Γ=95.28(3)°, V=1893.5(5) Å 3, Z=2, R=0.043 and R w=0.054 for 4501 reflections with I> 3σ( I). The anion [V 3S 7(Me 2dtc) 3] − is isostructural (exclusive of R groups in the ligand), but not isoelectronic with its Mo analogue [Mo 3S 7(Et 2dtc) 3] +, and has a lower mean oxidation state (+3 1 3 ) of vanadium than that observed in [V 3S 4(edt) 3] 3−. The structural parameters show the identity of three V atoms, implying an electronic delocalization. The 1H NMR spectrum exhibits two types of methyl resonances of the ligand at 10.69 and 8.72 ppm with an intensity ratio of 1:1.
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