By utilizing different small amine molecules as structure-affecting agents (SAAs) and charge-balancing agents (CBAs), four new MSnQ (M = Zn, Ag; Q = S, Se) compounds with the anionic architectures ranging from a one-dimensional (1D) chain to a three-dimensional (3D) network have been solvothermally synthesized. Compound (Me)(2)NH2(2)ZnSn3Se8 (1) features an anionic (4,4) layer of ZnSn3Se8(n)(2n) and represents a rare ZnSn3Se10T2 cluster-based two-dimensional ZnSnSe compound directed by organic amine. Compound NH4(3)AgSn3Se8 (2) contains infinite linear anionic chains of AgSn3Se8(n)(3n). Compound CH3NH3(2)H3OAg5Sn4Se12 center dot C2H5OH (3) exhibits a 3D open-framework structure of Ag5Sn4Se12(n)(3n) with intersecting 3D channels. Compound CH3NH3(6)Ag12Sn6S21 (4) features a 3D framework structure with 1D channels filled by CH3NH3(+) cations. The most fascinating structural feature of compound 4 is that a complex 3D Ag12S17(n)(22n) anionic network exists based on the combination of three types of basic building blocks of AgS2 dumbbells, AgS3 triangles, and AgS4 tetrahedra. The thermal stabilities, optical properties of the title compounds 14, as well as the theoretical band structure and density of states of compound 4 have been studied. Moreover, compound 3 displayed visible-light-driven photocatalytic activity for the degradation of crystal violet.
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