Synthesis and characterization of mononuclear bis[organohydrazido(2-)]molybdenum(VI) complexes. Crystal structures of [Mo(NNMePh)2(acac)2] and [Mo(NNPh2)2(acac)2]

Article abstract of DOI:10.1016/0020-1693(96)05096-7

In the presence of Na₂SO₄, 1-methyl-1-phenylhydrazine and 1,1-diphenylhydrazine react with [MoO₂(acac)₂] to yield [Mo(NNMePh)₂(acac)₂] (1) and [Mo(NNPh₂)₂(acac)₂] (2), respectively. Crystals of 1 are triclinic, space group P1, with unit cell dimensions a=9.780(6), b=11.134(11), c=13.504(7) A, α=110.69(6), β=95.71(5), γ=111.70(7)° and Z=2. The structure was solved using 4317 unique observed reflections; the refinement of 299 variables gave R and R_w values of 0.059 and 0.067, respectively. Crystals of 2 are monoclinic, space group C2/c, with unit cell dimensions a=21.151(3), b=13.174(3), c=13.477(2) A, β=123.17(1)° and Z=4. The structure was solved using 2760 unique observed reflections; the refinement of 195 variables gave R and R_w values of 0.039 and 0.040, respectively. In both complexes, the molybdenum atom displays distorted octahedral geometry with nearly linear cis-hydrazido ligands.