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The reaction of MOCl 4  (C 2 H 5 CN) 2  with (CH 3 ) 3 SiN 3  and subsequent addition of Na[HB(3,5-Me 2 pyz) 3 ] yields the nitrido azido complexes MoN(N 3 ) 2 [HB(3,5-Me 2 pyz) 3 ] and MoN(N 3 )Cl[HB(3,5-Me 2 pyz) 3 ]. The two complexes crystallize from toluene as mixed crystals (space group P2 1 /n, a = 1630.6, b = 878.0, c = 1675.5 pm, β = 112.67°, Z = 4). Crystallographic equivalent positions are occupied in a 4:1 ratio by diazido and monoazido monochloro complexes. The central Mo atom exhibits a sixfold coordination in form of a distorted octahedron with the nitrido ligand and one of the three pyrazol rings in axial positions. The triply bonded nitrido nitrogen atom (Mo≡N 164.2 pm) causes a strong trans effect, resulting in a long Mo-N6 bond (245 pm) to the trans positioned pyrazole nitrogen atom. The Mo-N distances in the equatorial plane are Mo-N2 215 and Mo-N4 216 pm, respectively. The nitrido complexes are remarkably stable against hydrolysis, probably due to steric shielding by the [HB(3,5-Me 2 pyz) 3 ] -  ligand. ν(Mo≡N) is observed at 1025 cm -1

zeitschrift für naturforschung b

Nitrido-Azido-Komplexe des Molybdän(VI): Synthese und Kristallstruktur von MoN(N 3 ) 2 [HB(3,5-Me 2 pyz) 3 ] und MoN(N 3 )Cl[HB(3,5-Me 2 pyz) 3 ] / Nitrido Azido Complexes of Molybdenum(VI): Synthesis and Crystal Structure of MoN(N 3 ) 2 [HB(3,5-Me 2 pyz) 3 ] and MoN(N 3 )Cl[HB(3,5-Me 2 pyz) 3 ]