Abstract
The diamagnetic complexes (n-Bu 4N) 4[PM 11O 39{Mo(NO)}] (M = Mo, W) have been synthesized in acetonitrile by reaction of the lacunary [PM 11O 39] 7− species, generated in situ through degradation of the patent complete Keggin anions by n-Bu 4NOH, with either (n-Bu 4N) 2[Mo 5O 13(OMe) 4(NO){Na(MeOH)}]·3MeOH or [Mo(NO)(OMe)(Me 2CNO) 2] 2 acting as a source of the [Mo(NO)] 3+ unit. These new nitrosyl-oxometalates have been characterized by elemental analysis, infrared spectroscopy, electrochemistry, and 31P and 183W spectroscopy. Comparison of electrochemical and spectral data of the nitrosyl derivatives to those of the parent Keggin anions demonstrate that the electron-withdrawing effect of the nitrosyl ligand is opposed to the overall increase in charge of the heteropolymetalate framework arising from the replacement of an MO 4+ unit by an [Mo(NO)] 3+ unit. In the case of [PW 11O 39{Mo(NO)}] 4−, 183W NMR data also support some delocalization of the Mo(II) d-electrons onto the polytungstate ligand.
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