The Hydrothermal Synthesis, Crystal Structures and Thermal Stability of the Novel One- and Two-Dimensional Thioantimonate(III) Compounds [Co(tren)]Sb2S4 and [Ni(tren)]Sb2S4

Abstract

Two novel thioantimonate(III) compounds [Co(C 6 H 18 N 4 )]-Sb 2 S 4 (1) and [Ni(C 6 H 18 N 4 )]Sb 2 S 4 (2) were synthesised under solvothermal conditions by reacting the transition metal, Sb and S in a 50% solution of tris(2-aminoethyl)amine (tren). The use of a tetradentate amine yields incompletely shielded transition metal cations which in turn are able to form bonds to the sulfur atoms of thioantimonate(III) anions. Compound 1 crystallises in the orthorhombic space group Pbca, a = 13.886 (3) Å , b = 11.452(2) Å , c = 20.549(4) Å , V = 3268(1) Å 3 , Z = 8 and compound 2 crystallises in the monoclinic space group P2 1 /n, a = 6.906(1) Å , b = 22.822(5) Å , c = 10.347(2) Å , β = 103.17(3)°, V = 1587.9(6) Å 3 , Z = 4. The 2 ϰ [Sb 2 S 4 2−] anion in compound 1 is formed by an SbS 3 and an SbS 4 unit sharing a common corner. Two SbS 4 units have a common edge to form an Sb 2 S 2 heterocycle. Four such Sb 2 S 2 rings are at the corners of a two-dimensional square-like net. Interconnection of the rings by SbS 3 pyramids yields Sb 10 S 10 rings with pores measuring 10·8.4 Å in diameter. The pores are filled by the [Co(tren)] 2+ cations. The [Co] 2+ cation is in a trigonal

The Effect of Temperature onto the Crystal Structure of Thioantimonates: Solvothermal Syntheses and Crystal Structures of [Co(dien)2][Co(tren)SbS4]2·0.5H2O and {[Co(tren)]2[CoSb2S6]}·H2O

“…Such an elongation of a bond can be explained with the so-called trans-effect. The Co(1)-S(1) bond at 2.3701(8) Å is in the range of data published in literature [54,55]. The angles around the Co (1) 2+ cation suggest an appreciable distortion ( Table 2).…”

“…The Co (2) 2+ cation is octahedrally surrounded by two tridentate dien ligands in the s-fac-configuration. The Co(2)-N bond lengths between 2.153(4) and 2.192(5) Å are in the range found in other Co amine compound [54][55][56]. The angles around Co (2) 2+ (Table 2) Table 1).…”

Solvothermal synthesis and crystal structure of Sb(III) and Sb(V) thioantimonates: [Mn(en)3]2Sb2S5 and [Ni(en)3(Hen)]SbS4

“…In recent years, a large number of thioantimonates(III) with organic cations [1][2][3][4], transition metal complex cations [5][6][7][8][9][10][11][12][13][14][15][16][17][18] and other cations [19,20] serving as counterions to Sb x III S y nÀ anions, have been synthesized under hydro-or solvo-thermal conditions. The rich structural diversity of thioantimonates(III) results from variable coordination behaviors of Sb(III) atom caused by the stereochemically active lone pair [21].…”

Solvothermal syntheses, crystal structures, and properties of new lanthanide compounds based on tetraselenidoantimonate and tetraethylenepentamine mixed ligands

“…ions to form TM-S or TM-Se bond with the chalcogenidoantimonate anions. As a result, ternary TM-chalcogenidoantimonates were obtained [30][31][32][33][34][35][36][37][38].…”