The novel tridentate ligand in 1 was generated by head‐to‐head coupling and double insertion of PhC≡CH into the Rh−O bond of [(η5‐C5Me5)RhCl{PPh2(2‐O‐6‐MeOC6H3)}]. Propargylic esters (Me, Et) undergo single insertion to give seven‐membered metallacycles.
A new series of N 2 O tridentate ligands HL n (n ) 2-5) have been prepared through N-methylation or N-benzylation of 2-N-(2-pyridylmethyl)aminophenol (HL 1 ). Treatment of these ligands with WO 2 Cl 2 (DME) (DME ) 1,2-dimethoxyethane) in the presence of triethylamine leads to the formation of cis-dioxotungsten(VI) complexes WO 2 (L n )Cl (n ) 1-5). Reaction of WO 2 (L 1 )Cl with Me 3 SiCH 2 MgCl gives the alkyl derivative WO 2 (L 1 )-(CH 2 SiMe 3 ), which has been structurally characterized.
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