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Five quaternary Nb-containing sulfides Rb 2 CuNbS 4 (1), Rb 2 AgNbS 4 (2), Cs 2 AgNbS 4 (3), RbCu 2 NbS 4 (4), and CsCu 2 NbS 4 (5) were synthesized under solvothermal conditions by using Nb powder as the initial material, and compounds 1 – 3 exhibit excellent photoelectric response properties. [Display omitted] • Five Nb-containing quaternary sulfides were synthesized by using Nb power as the initial material. • This is the first time that a mild solvothermal method was used in the preparations of Nb-containing sulfides. • Compounds 1 – 3 exhibit excellent photoelectric response properties. Five quaternary sulfides in the A-Cu/Ag-Nb-S (A = Rb, Cs) family, namely Rb 2 CuNbS 4 (1), Rb 2 AgNbS 4 (2), Cs 2 AgNbS 4 (3), RbCu 2 NbS 4 (4), and CsCu 2 NbS 4 (5) have been synthesized by using Nb powder as the initial material under mild solvothermal conditions. Compounds 1 – 3 crystallize in space group Fdd and possess one-dimensional (1D) infinite [MNbS 4 ] n 2n– (M = Cu for 1 ; Ag for 2 and 3) anionic chains formed by edge-sharing of [MS 4 ] (M = Cu, Ag) and [NbS 4 ] units. Compounds 4 – 5 are isostructural and crystallize in space group Ama 2. Their structures contain the two-dimensional (2D) [Cu 2 NbS 4 ] n n– anionic layers, which can be regarded as a further extension of the [CuNbS 4 ] n 2n– anionic chains in compounds 1 – 3. The optical bandgaps and photoelectric response performances of these compounds have also been investigated. [ABSTRACT FROM AUTHOR]