On the complex hedgehog-shaped cluster species containing 368 Mo atoms: Simple preparation method, new spectral details and information about the unique formation

Abstract

The compound Na48[HxMo368O 1032(H2O)240(SO4) 48]·ca. 1000H2O ≡ Na48 1a·ca. 1000H2O (1) exhibiting an unusual nanosized hedgehog-type cluster anion, has been obtained in good yield. 1 was characterized by elemental analysis thermogravimetry and spectroscopic methods. Information about unusual aspects of the formation is reported. The deep-blue compound Na48[HxMo368O1032(H 2O)240(SO4)48]·ca. 1000H 2O ≡ Na48 1a·ca. 1000H2O (1) exhibiting an unusual nanosized hedgehog-type cluster anion, could now be obtained in good yield - allowing now several materials science studies - in the presence of a high concentration of an electrolyte destroying the hydration shell, in only two days. 1 was characterized by elemental analysis (including redox titrations to determine the (formal) number of MoV centers), thermogravimetry and spectroscopic methods (IR, resonance Raman, Vis/NIR). Information about unusual aspects of the formation is reported together with additional spectroscopic details as well as a new crystal structure determination of the very complex system while confirming the earlier one. © 2004 Elsevier Ltd. All rights reserved.