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The new thioantimonate(III) (C 6 N 2 H 18 )Sb 4 S 7  (C 6 N 2 H 16  = 1,6-diaminohexane) was synthesized under solvothermal conditions using Sb, S and 1,6-diaminohexane (1,6-DAH). The compound crystallizes as orange needles in the triclinic space group P1̅ with lattice parameters a = 6.9834(5), b = 11.8748(10), c = 13.6588(12) Å , α = 115.248(9), β = 100.165(9) and γ = 92.568(9)°. A central SbS 4  group shares edges with two other SbS 4  moieties forming Sb 3 S 8  units which are joined by SbS 3  pyramids sharing vertices to form a chain of alternating Sb 3 S 8  and SbS 3  units. One S atom of the SbS 3  pyramid connects neighboring chains into sheets which contain large Sb 10 S 10  heterorings. The sheets are then further connected into four atoms thick double sheets. Six edge-linked SbS4 units are condensed yielding a complex Sb 6 S 14  building block. Layers of diprotonated amines and thioantimonate( III) layers are stacked along [001] in a sandwich-like fashion with an interlayer distance of 8.46 Å . The amine layer is two molecules thick with the amines being oriented parallel to the anionic layers. The title compound represents the first example for a layered [Sb 4 S 7 ] 2−  anion with a diamine as structure director. The compound is an optical semiconductor with a band-gap of about 1.9 eV

(C 6 N 2 H 18 )Sb4S7 a Thioantimonate(III) with a Layered [Sb4S7]2– Anion in the Presence of a Diprotonated Amine as Structure Director