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By using a new type of lacunary tungstoselenite {Se2W29O103} (1), which contains a “defect” pentagonal {W(W)4} unit, we explored the assembly of clusters using this building block and demonstrate how this unit can give rise to gigantic nanomolecular species, using both a “one-pot” and “stepwise” synthetic assembly approach. Specifically, exploration of the one-pot synthetic parameter space lead to the discovery of {Co2.5(W3.5O14)(SeW9O33)(Se2W30O107)} (2), {CoWO(H2O)3(Se2W26O85)(Se3W30O107)2} (3), and {Ni2W2O2Cl(H2O)3(Se2W29O103) (Se3W30O107)2} (4), effectively demonstrating the potential of the {Se2W29} based building blocks, which was further extended by the isolation of a range of 3d transition metal doped tetramer family derivatives: {M2WnOm(H2O)m(Se2W29O102)4} (M = Mn, Co, Ni or Zn, n = 2, m = 4; M = Cu, n = 3, m = 5) (5 - 9). To contrast the ‘one-pot’ approach, an optimized stepwise self-assembly investigation utilizing 1 as a precursor was performed showing that the high nuclearity clusters can con...

A new family of TeIV-containing heteropolyoxometalate building blocks which consist of a {W3} top unit and one, two, and three layers of {TeW6} base units in [TeW9O33]8-, [Te2W15O54]10-, and [Te3W21O75]12-, respectively, is synthesized.