SYNTHESIS, CHARACTERIZATION AND X-RAY CRYSTAL-STRUCTURE OF (H2B(ME2C3N2H)2)MOIVO(S2PPRI2)

Reaction Of MOO(S2PPri2)2 and K{H2B(Me2C3N2H)2} in refluxing toluene p roduces green, diamagnetic, air-stable {H2B(Me2C3N2H)2}MO(IV)O(S2PPri2 ) (1), which has been characterized by analytical, mass spectrometric, infrared and n.m.r. spectroscopic, and X-ray crystallographic techniq ues. Crystals of (1) are triclinic and belong to space group P1BAR, wi th a 10.289(1), b 13.601(2), c 8.737(1) angstrom, alpha 94.31(l), beta 107.71(l), gamma 79.56(1)-degrees, V 1145.2 angstrom3 and Z 2. The st ructure was solved by Patterson and Fourier methods and refined by usi ng 3631 reflections to a final R value of 0-024 (R(w) 0.041). The five -coordinate square pyramidal complex is composed of apical terminal ox o [Mo-O(1) 1-658(2) angstrom] and bidentate H2B(Me2C3N2H)2-and S2PPri2 - ligands coordinated to molybdenum. Ferrocenium oxidation of (1) prod uces the mononuclear molybdenum(v) complex [{H2B(Me2C3N2H)2}MOVO(S2PPr i2)]+ (e.p.r.: g 1.964, a(Mo-95, Mo-97) 41.7 x 10(-4) cm-1, a (P-31) 3 0.1 X 10(-4) CM-1).