96394-41-1Relevant academic research and scientific papers
Synthesis and structure of a seven-coordinate molybdenum carbonyl fluoride derivative: [Et4N][Mo(CO)2(S2CNEt2) 2F]
Burgmayer,Templeton
, p. 2224 - 2230 (2008/10/08)
An improved preparative route into molybdenum(II) and tungsten(II) dithiocarbamate chemistry has been developed that proceeds through [M(CO)5I]- and [M(CO)4I3]-. Addition of fluoride or azide ion to M(CO)2(S2CNR2)2 (M = Mo, W) yields [M-(CO)2X(S2CNR2)2]- (X = F, N3). The structure of [Et4N][Mo(CO)2(S2CNR2)2F] (1), a rare molybdenum(II) carbonyl fluoride complex, is reported with crystallographic parameters of a = 11.152 (4) ?, b = 16.039 (5) ?, c = 15.846 (4) ?, β = 91.91 (2)°, and Z = 4 defining a monoclinic lattice of space group P21/n. Refinement to R1, = 4.7% and R2 = 3.4% was attained. The idealized geometry of 1 is that of a capped trigonal prism where fluoride occupies the capping site trans to both carbonyl groups. The structure of 1 exhibits an acute OC-M-CO angle of 67.4°, and extended Hückel calculations on Mo(CO)2(S2CNR2)2 (OC-M-CO = 74.3°) and the fluoride complex 1 have been performed to probe factors that influence this angle.
