Abstract
Novel tetranuclear vanadyl glycollates [Ni(phen)3]2[VIV4O4(glyc)6]·23H2O (1) and [Ni(phen)3]2[VIV4O4(glyc)6]·16H2O (2) have been obtained through the capture of bulky nickel phenanthroline cation (H2glyc=glycollic acid, phen=1,10-phenanthroline), and the mixed-ligand complex [VIV4O6(glyc)2(bpy)4]·6H2O (3) (bpy=2,2′-bipyridine) was isolated with the addition of bpy under hydrothermal condition. Tetrameric 1 and 2 are easily oxidized to dimeric complex [Ni(phen)3][VV2O4(glyc)2]·5H2O (4), while 3 with bipyridine is stable. The degradation process was traced by IR and XRD experiment. 1–4 feature bidentate glycollate that chelates to vanadium atom through α-alkoxy and α-carboxy groups, which were full characterized by elemental analysis, TG, IR, UV–Vis, EPR, XRD and X-ray structural analyses. Bond valence calculation is also performed.
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