| Chalcogenidogermanate [GexQy]n- (Q = S, Se and Te) materials have been a research field with rapid expansion in the past decades, mainly because of their rich structural chemistry and potential applications in ion exchange, adsorption, semiconductors, photoluminescent, magnetic and others. Solvthermal synthesis of metal chalcogenide is a simple and effective method, a series of chalcogenido- germanates, thioarsenes and thiostannates were prepared by this method in the presence of transition metal complexes as structure-directing agent and characterized by elemental analysis, fluorescence spectroscopy,thermogravimetric analysis , IR spectroscopy , powder X-ray diffraction, single crystal X-ray diffraction X-ray crystallographic and the solid UV absorption spectroscopy. In this paper, the main four aspects are as followes:1. Four dimeric chalcogenidogermanates [Co(en)3]2Ge2S6 (1), [Ni(dien)2]2Ge2S6(2), [Fe(dien)2][H2dien]Ge2S6(3) and [Co(dien)2][H2dien]Ge2S6(4) have been solvothermally synthesized by using different organic en or dien as structure-directing agents respectively. The different cations as structure directing agents have a significant influence on the arrangement of [Ge2S6]4- anions.2. Four adamantane-like cluster chalcogenidogermanates [Co(dap)3]2Ge4S10Cl2(5),[Co(dap)3]2Ge4S10Cl2(6),[Ni2(μ-teta)(teta)2]Ge4S10 H2O(7), and [Ni(teta)2]2Ge4Se10·0.5H2O(8) were synthesized by solvothermal method in dap or teta. The structural feature of these compounds possesses discrete [Ge4Q10]4-(Q = S, Se) adamantane-like anions combined with metal complexes.3. Two thioarsenes [Co(dien)2]2As3S6(9) and [Mn2(teta)2]As2S5(10) were synthesized by solvothermal method in dien or teta. The [Co(dien)2]2+ cations in 9 have two different optical isomer, while the [Mn(teta)]2As2S5 moieties in 10 built up from saddle-like [As2S5]4- anions as a tetra-dentate bridging ligand connecting two [Mn(teta)]2+ groups via terminal S atoms. 4. Two thiostannates [Co(dien)2](H2dien)Sn2S6 (11) and [Zn(tren)]2Sn2S6 (12) were made under solvothermal conditions. Both 11 and 12 contain dimeric [Sn2S6]4- anion built up from two SnS4 tetrahedra sharing a common edge. The different cations act as structure directing agents have a significant influence on the arrangement of [Sn2S6]4- anions.
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