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Solvothermal Synthesis and Crystal Structures of Two Thioantimonate(V) Compounds with the [SbS 4 ] 3— Anion Acting as a Monodentate Ligand: [Mn(C 6 H 18 N 4 )(C 6 H 19 N 4 )]SbS 4 and [Mn(C 6 H 14 N 2 ) 3 ] 2 [Mn(C 6 H 14 N 2 ) 2 (SbS 4 ) 2 ]·6H 2 O
Author(s) -
Schaefer Michael,
Engelke Lars,
Bensch Wolfgang
Publication year - 2003
Publication title -
zeitschrift für anorganische und allgemeine chemie
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.354
H-Index - 66
eISSN - 1521-3749
pISSN - 0044-2313
DOI - 10.1002/zaac.200300158
Subject(s) - denticity , triclinic crystal system , monoclinic crystal system , octahedron , chemistry , crystallography , crystal structure , ligand (biochemistry) , molecule , protonation , stereochemistry , amine gas treating , ion , organic chemistry , receptor , biochemistry
The two novel thioantimonate(V) compounds [Mn(C 6 H 18 N 4 )(C 6 H 19 N 4 )]SbS 4 ( I ) and [Mn(C 6 H 14 N 2 ) 3 ] 2—[Mn(C 6 H 14 N 2 ) 2 (SbS 4 ) 2 ]·6H 2 O ( II ) were synthesized under solvothermal conditions by reacting elemental Mn, Sb and S in the stoichiometric ratio in 5 ml tris(2‐aminoethyl)amine (tren) at 140 °C or chxn ( trans ‐1, 2‐diaminocyclohexane, aqueous solution 50 %) at 130 °C. Compound I crystallises in the triclinic space group P 1¯, a = 9.578(2), b = 11.541(2), c = 12.297(2)Å, α = 62.55(1), β = 85.75(1), γ = 89.44(1)°, V = 1202.6(4)Å 3 , Z = 2, and II in the monoclinic space group C 2/c, a = 32.611(2), b = 13.680(1), c = 19.997(1)Å, β = 117.237(5)°, V = 7931.7(8)Å 3 , Z = 4. In I the Mn 2+ cation is surrounded by one tetradentate tren molecule, one protonated tren acting as a monodentate ligand and a monodentate [SbS 4 ] 3— anion yielding a distorted octahedral environment. In II one unique Mn 2+ ion is in an octahedral environment of three bidentate chxn molecules and the second independent Mn 2+ ion is coordinated by two chxn ligands and two monodentate [SbS 4 ] 3— units leading to a distorted octahedral surrounding. The compounds were investigated and characterized with thermal and spectroscopic methods.