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A new compound, K 5 [(Mo 3.2 W 1.8 )O 11 ](PO 4 ) 3 [(P 0.5 Mo 0.5 )O 4 ], was synthesized via solid-state reaction and its crystal structure was determined by single-crystal X-ray diffraction. This compound crystallizes in the space group  Pnma , with  a  = 9.0360(4) Å,  b  = 10.1603(4) Å,  c  = 26.1538(12) Å and  V  = 2401.14(18) Å 3 . The structure consists of a corner-sharing MO 6 –TO 4  (M = Mo, W; T = P, Mo) polyhedral connection arranged to form an ordered packing of ∼14.9 Å-thick layers parallel to (001). The stacking of the layers forms trigonal, tetragonal and hexagonal channels. XPS study reveals the presence of W at the hexavalent state only, whereas Mo appears as a mixed-valent species (Mo 6+ , Mo 5+  and Mo 4+ ). Magnetic susceptibility reveals the occurrence of a relevant antiferromagnetic coupling and is consistent with the presence of reduced metal species as indicated by the XPS results.

A new layered potassium-based molybdenum–tungsten monophosphate: synthesis, crystal structure, XPS and magnetic studies