A Triangular [Mo₃S₇]⁴⁺Complex: Tris(diethyldithiocarbamato-S,S')tris(μ₂-η²-disulfido)(μ₃-sulfido)trimolybdenum(IV)(3Mo—Mo)Diethyldithiocarbamate

Abstract

In the cluster cation of the title compound, [Mo3S7-(Et2NCS2)3](Et2NCS2), three Mo atoms form an approximately equilateral triangle, with Mo---Mo distances ranging from 2.7140(5) to 2.7277 (5).4,, and Mo--Mo---Mo angles of ca 60 °. The triangle is capped by the/z3-S atom, and each Mo---Mo bond is bridged by a disulfido group in #2-772 mode. Diethyldithiocarbamate ligands (Et2dtc) are chelated to the Mo atoms with an average S--Mo--S bite angle of 69.98 (1) °. There is a weak S-.-S interaction between the cluster cation and the anion (Et2dtc-). CommentCompounds containing the [MOBS7] ~ core have been studied extensively (Miiller et al., 1979;Keck et al.,

Reactivity of the [Mo3(μ3-S)(μ2-S2)3Br6]2- Anion toward the Imidodiphosphinochalcogenido Ligands [N(QPPh2)2]- (Q = S, Se): Synthesis and Characterization of [Mo3(μ3-S)(μ2-S2)3{N(QPPh2)2}3]Br

“…Bond distances (Table 2) and angles in these compounds are unexceptional. The mean Mo-Mo distances (Table 2) are in agreement with those in other Mo 3 clusters (range 2.719(2) Å-2.757(1) Å) [29][30][31] and are consistent with Mo-Mo singlebond lengths. 32,33 Each S eq atom of the µ 2 -S 2 2ligand is essentially in the Mo 3 plane, deviating by less than 0.2 Å.…”

“…Physical Measurements. 31 P NMR spectra were recorded on samples in 5 mm tubes on a 300 MHz Gemini Routine apparatus operating at 121.47 MHz in the Fourier transform mode. Chemical shifts are referenced to an external 85% H3PO4 solution.…”

“…Found: C, 38.29; H, 2.89; N, 1.62 (solvent molecules are apparently lost in preparation for chemical analyses.) 31 P-{ 1 H} NMR (ppm, CH2-Cl2/CD2Cl2, 295 K): δ 31.10 (s, 1), 30.24 (s, 1). UV-vis (nm, CH2-Cl2): 419 ( ) 1420 M -1 cm -1 ), 367 ( ) 2480 M -1 cm -1 ).…”