Thioantimonate chemistry is characterized by a fascinating structural and chemical diversity. 1 One intriguing structural feature is that for a given Sb/S ratio the dimensionality of the thioantimonate anion may range from zero-dimensional (0D) isolated anions to three-dimensional (3D) networks. Analyzing the thioantimonate(III) structures containing charge compensating cations of different sizes and charges, only a moderate influence on the dimensionality could be identified. For instance, 0D Ni 2+ containing thioantimonates(III) were obtained with diethylenetriamine (dien) as solvent; one-dimensional (1D) chains with ethylenediamine (en), dien, and tris(2-aminoethyl)amine (tren); two-dimensional (2D) layers with 1,2-diaminopropane (1,2-dap), dien, and tren; and 3D networks with en, dien, and 1,4,8,11-tetraazacyclotetradecane (cyclam). This clearly demonstrates that the choice of the size/charge of the solvent/structure director has no effect on the dimensionality of the inorganic part of the compounds. There are no general rules allowing prediction of the chemical composition and/or crystal structure of thioantimonates formed under solvothermal conditions. Thiometallate compound formation was investigated by us applying in situ X-ray scattering and X-ray absorption techniques demonstrating the complexity of the reactions occurring under solvothermal conditions. 2À5 Concerning the structural chemistry of thioantimonates containing Ni-amine complexes as structure directing and charge balancing agents, two compounds are 0D, namely, [Ni (dien) 2 ]-Sb 4 S 8 6 and [Ni(dien) 2 ] 3 (Sb 3 S 6 ) 2 . 7 In the former compound, four SbS 3 moieties share common corners to form the [Sb 4 S 8 ] 4À heterocycle. 6 The [Sb 3 S 6 ] 3À anion 7 is constructed by three vertex-linked SbS 3 pyramids. Several isolated thioantimonate(V) anions could also be isolated like [Ni(en) 3 ] 3 (SbS 4 )(NO 3 ), 8 [Ni-(dien) 2 ] 3 (SbS 4 ) 2 , 9 (paH)[Ni(tren)SbS 4 ], 10 [Ni(chxn) 3 ] 3 (SbS 4 ) 2 3 4H 2 O 11 and [Ni(en) 3 (enH)]SbS 4 . 12 Only in (paH)[Ni(tren)-SbS 4 ] 10 the Ni 2+ ion is octahedrally surrounded by four N atoms of the amine and by two S atoms of the [SbS 4 ] 3À anion. 1D chain anions are found in [Ni(tren)]Sb 2 S 4 , 13 [Ni(dien) 2 ]Sb 4 S 9 , 14 [Ni(tren)Sb 4 S 7 ], 15 [Ni(en) 3 ]Sb 2 S 4 , and [Ni(en) 3 ]Sb 4 S 7 . 16 The compound [Ni(tren)]Sb 2 S 4 13 is a rare example where the Ni 2+ ion is incorporated in the thioantimonate network via NiÀS bonds. ABSTRACT: The new thioantimonates [Ni(aepa) 2 ] 3 Sb 6 S 12 (1), [Ni(aepa) 2 ] 6 -(Sb 3 S 6 ) 2 (SO 4 ) 3 3 2H 2 O (2), and [Ni(aepa) 2 ]Sb 4 S 7 (3) (aepa = C 5 H 15 N 3 = N-(aminoethyl)-1,3-propandiamine) were obtained under solvothermal conditions by slightly varying the reaction conditions. In all compounds the [Ni(aepa) 2 ] 2+ complexes were formed in situ during the chemical reactions. Compound 1 features the new unique [Sb 6 S 12 ] 6À cyclic anion composed by vertex-linked SbS 3 trigonal pyramids. This [Sb 6 S 12 ] 6À cyclic anion represents the largest isolated thioantimon...

Unveiling the nanostructure of ball-milled MoS2 on different length scales by analyses of X-ray data, UV-Vis spectra and TEM images.

Carbon containing nano-sized molybdenum sulfide composites (MoS(x)C(y)) obtained by thermal decomposition reactions of (R(4)N)(2)MoS(4) (R = -H (C(0)), -CH(3) (C(1)), -C(3)H(7) (C(3)), and -C(6)H(13) (C(6))) show promising performance in visible-light driven photocatalytic hydrogen generation.