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Tetraphenylphosphonium tetrathiometalates, (PPh 4 ) 2 MS 4  (M = Mo, W), react with MoO 2  (acac) 2  (2:1) in boiling acetonitrile in redox processes to give mixed-crystal compounds (as expected) of the approximate composition (PPh 4 ) 2 [Mo 3 O 1.9 S 8.1 ] (1) and (PPh 4 ) 2 [Mo 1.4 W 1.6 O 1.3 S 8.3 ] (2), respectively. and  2  were characterized by single crystal X-ray structure analyses. The various anions o f 1 and  2  contain {M VI (μ-S) 2 Mo IV O (μ-S ) 2 M VI } cores (M = Mo (1); Mo, W  (2);  bond angle M ··· Mo ··· M = 151.3° (1) 152.2 - 154.3°  (2)),  which have high formation tendencies. The terminal positions are occupied by S and O atoms. The trinuclear anions of 1 correspond to the type [XYMo(μ-S) 2 MoO(μ-S) 2 MoSX ] 2-  (X = O, S; Y = S, S 2 ). In 2 there are two sets of anions of the type [XYM(μ-S) 2 MoO(μ-S) 2 WS 2 ] 2-  and [ZSM (μ-S) 2 MoO(μ-S) 2 MZS] 2-  (Z = S n /O m ) in the ratio o f 2:1, occupying two symmetry-independent sites in the unit cell. Complex 2 is the first structurally characterized mixed-metal Mo - W thiometalate.

zeitschrift für naturforschung b

The Reactions of Dioxobis(acetylacetonato)moIybdenum, MoO 2 (acac) 2 , with Tetrathiomolybdate and Tetrathiotungstate. High Formation Tendency of the {M vi (μ-S) 2 M iv } (μ-S ) 2 M VI } Group and the [M VI ,S 3 (S 2 )] 2 - Type Ligand (M = Mo, W)