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Withdifferent transition metal (TM) complexes as structure-directingagents or structure-building units, a series of new mercury thioantimonateswith abundant architectures ranging from one-dimensional (1D) ribbonsto two-dimensional (2D) layers have been solvothermally synthesizedand structurally characterized. Compounds [Co(en)3]Hg2Sb2S6(1) (en = ethylenediamine)and [Ni(1,2-dap)3]2HgSb3S7Cl (2, 1,2-dap = 1,2-diaminopropane) containa discrete 2D [Hg2Sb2S6]n2n–layer and1D [HgSb3S7]n3n–chain, respectively. Compounds[Ni(1,2-dap)3]HgSb2S5(3) and [Mn(dien)2]HgSb2S5(4, dien = diethylenetriamine) feature distinct 2D[HgSb2S5]n2n–layer and 1D [HgSb2S5]n2n–ribbon, respectively, whereas the 1D [HgSb2S5]n2n–chains are attached by [TM(tren)]2+complexes via TM–Sbonds to form 1D {[TM(tren)]HgSb2S5}nribbons in compounds [TM(tren)]HgSb2S5(TM = Mn (5), Fe (6), Co(7), tren = tris(2-aminoethyl)amine). Compounds [TM(dien)2]Hg3Sb4S10(TM = Mn (8), Co(9), Ni(10)) feature 2D [Hg3Sb4S10]n2n–anionic layers separated by[TM(dien)2]2+cations. The most interestingstructural feature of these compounds is the presence of three differenttypes of coordination environments of Hg centers including linear[HgS2] unit, [HgS3] triangle, and [HgS4] tetrahedron. The optical properties and thermal stabilities ofthe title compounds were studied by UV–vis spectra and thernogravimetricanalyses, respectively. The photocatalytic experiments indicated that 3, 4, and 10were able to degraderhodamine B (RhB) under visible irradiation. [ABSTRACT FROM AUTHOR]