RESEARCH ARTICLE · Journal of the Chemical Society Dalton Transactions · 1997

Bis[hydrazido(2−)] and related complexes of molybdenum(VI): towards alkene-metathesis catalysts based on hydrazido(2−) ligation

J.R. Dilworth, Vernon C. Gibson, Can‐Zhong Lu, John R. Miller, Carl Redshaw, Yifan Zheng

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Abstract

The complex [Mo(NBu t ) 2 Cl 2 (dme)] (dme = 1,2-dimethoxyethane) underwent an imide-ligand exchange reaction with an excess of 1,1-diphenylhydrazine hydrochloride in refluxing dme to give the bis[hydrazido(2-)] complex [MoCl 2 (NNPh 2 ) 2 (dme)] 1. Reaction of 1 with an excess of PMe 3 in CH 2 Cl 2 gave [MoCl 2 (NNPh 2 ) 2 (PMe 3 ) 2 ] 2. Treatment of Na 2 [MoO 4 ] with 2 molar equivalents of Ph 2 NNH 2 ·HCl in the presence of NEt 3 and SiMe 3 Cl in refluxing dme afforded the salt [NHEt 3 ][MoCl 4 (NNPh 2 )(NHNPh 2 )] 3. The crystal structures of 1–3 have been determined; all possess octahedral geometries with unidentate hydrazido groups. The hydrazido(2-) Mo–N bond distances vary from 1.749(2) and 1.771(2) Å in 1, to 1.793(3) in 2 and 1.748(2) Å in 3, with no simple correlation with the Mo–N α –N β angle. The anionic component of 3 contains a bent hydrazide(1-) ligand (Mo–N–N 136.0°) and a linear hydrazido(2-) group (Mo–N–N 174.4°).

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