Synthesis and reactivity of bis(3,5-dimethylpyrazol-1-yl)ethane tetracarbonylmolybdenum and tungsten X-ray crystal structureof bis(3,5-dimethylpyrazol-1-yl)ethane tetracarbonyltungsten

Bis(3,5-dimethylpyrazol-1-yl)ethane tetracarbonylmolybdenum (1a) and tungsten (1b) have been synthesized by the direct reaction of bis(3,5-dimethylpyrazolyl)ethane (bmpze) with M(CO)6 (M = Mo or W). The molecular structure (1b), determined by x-ray crystallography, showed the seven-membered ring W–N–N–C–C–N–N to be in the boat conformation. Upon treatment with RSnCl3 (R=Ph or Cl) in CH2Cl2 at room temperature, complexes (1a) and (1b) gave the seven-coordinate oxidative-addition products [(bmpze)M(CO)3(SnCl2R)Cl] [M = Mo, R = Ph, (2a); M = W, R=Ph, (2b); M = Mo, R = Cl, (2c); M = W, R = Cl, (2d)]. When complexes (1b) and (2b) were heated under reflux with 1,2-bis(diphenylphosphino)ethane (dppe), the ligand, bmpze, in these complexes was easily removed. The novel compounds were characterized by 1H-n.m.r., i.r. and elemental analysis.