Metal chalcogenides, as a new class of semiconductor materials, have a broad range of applications in synthetic chemistry due to their rich structures and excellent properties. We have synthesized two selenoantimonates A4Zn2Sb2Se7 [A = Rb(1), Cs(2)] under solvothermal conditions in the visible region using a band gap optimization strategy with alkali metals as structure-directing agents. Compounds 1 and 2 have a two-dimensional layered structure consisting of charge-balanced Rb+(1) or Cs+(2) cations and [Zn2Sb2Se7]4− anions with novel 20-membered rings (20-MR) [Zn6Sb4Se10] with an aperture of 5.6949 × 13.7741 Å2 formed in the middle. Furthermore, we have investigated the crystal structure, band gap, photoelectronic properties, and energy band structure.
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