A new compound, K5[(Mo3.2W1.8)O11](PO4)3[(P0.5Mo0.5)O4], 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) Å3. The structure consists of a corner-sharing MO6–TO4 (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 (Mo6+, Mo5+ and Mo4+). 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.

中文翻译：

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新型层状钾基单磷酸钼钨：合成、晶体结构、XPS 和磁性研究

一种新化合物，K5[(莫3.2瓦1.8)O11](PO4）3[(P0.5莫0.5)O4]，通过固相反应合成，并通过单晶X射线衍射测定了其晶体结构。该化合物在空间群中结晶普马， 和A= 9.0360(4) 埃,乙= 10.1603(4) 埃,C= 26.1538(12) 埃 和V= 2401.14(18) 埃3。该结构由一个共享角的MO组成6-到4(M = Mo, W; T = P, Mo) 多面体连接排列形成平行于 (001) 的约 14.9 Å 厚层的有序堆积。层的堆叠形成三角形、四边形和六边形通道。XPS 研究揭示 W 仅以六价态存在，而 Mo 则以混合价态出现（Mo6+, 钼5+和莫4+）。磁化率揭示了相关反铁磁耦合的发生，并且与 XPS 结果表明的还原金属物质的存在一致。