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

The deep-blue compound Na<SUB>48</SUB>[H<SUB>x</SUB>Mo<SUB>368</SUB>O<SUB>1032</SUB>(H<SUB>2</SUB>O)<SUB>240</SUB>(SO<SUB>4</SUB>)<SUB>48</SUB>] · ca. 1000H<SUB>2</SUB>O = Na48 1a · ca. 1000H<SUB>2</SUB>O (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 Mo<SUP>V</SUP> 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