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  • Author: Wolfgang Bensch x
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Abstract

The reaction of manganese with antimony and sulfur in an aqueous ethylenediamine (en) solution under hydrothermal conditions gives Mn(en)3Sb4S7. The structure of the title compound consists of Mn(en)3 2+ cations and infinite one-dimensional (Sb4S7 2-)„ anions forming slabs via long secondary interchain Sb···S bonds. A comparison between phases with polymeric (Sb4S7 2- )„ anions shows in general a trend towards a lower dimensionality of the thioantimonate assembly with increasing cation size. In the title compound the lowest number of interchain Sb···S interactions is observed among other phases with chainlike Sb4S7 2- anions.

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Abstract

Single crystals of slightly hygroscopic barium nitrite Ba(NO2)2 were prepared by thermal decomposition of barium nitrite monohydrate and subsequent recrystallization in a solution of methanol and p-xylene. The compound crystallizes in the orthorhombic space group P212121 with a = 7.6331(16) Å, b = 8.3671(36) Å, c = 6.7336(8) Å and Z = 4. The structure was determined from X-ray intensities measured on a four-circle diffractometer and refined to R = 0.035 and wR = 0.048. The barium atoms exhibit an elevenfold coordination made up by nine oxygen atoms within distances ranging from 2.776(6) Å to 3.010(6) Å and two nitrogen atoms within distances of 3.059(7) Å and 3.125(7) Å. Values for the O – Ba – O angles range from 41.5(2)° to 151.1(2)°. The N – O distances are in the range 1.236(9) to 1.265(8) Å.

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Abstract

The new compound {Mn(dien)2}2[MnSb2S7] (dien = diethylenetriamine) was obtained under solvothermal conditions and crystallizes in the orthorhombic space group Pbca. The main structural motif is the [MnSb2S7]4– anion being constructed by a [MnS4]6– tetrahedron, a [SbIIIS3]3– and a [SbVS4]3– anion. Each thioantimonate anion shares one edge with the Mn2+ centered cation generating the [MnSb2S7]4– unit. The two independent Mn2+ cations in the two {Mn(dien)2}2+ complexes are in a distorted octahedral environment of two tridentate acting dien molecules. One cation displays the λδλλ-conformation and the other the δλλδ-conformation. Several intermolecular S···H—N bonding interactions are found between the cations and the anions.

Abstract

The title compound has been synthesized under solvothermal conditions by the reaction of elemental chromium, antimony and selenium in a solution of 40% 1,2-ethanediamine (en) in methanol. The crystal structure consists of tetrahedral SbSe4 3- anions which are connected by monoprotonated 1,2-ethanediamine (enH+) cations via N-H--Se hydrogen bonding. The enH+ cations are joined via strong N-H -N hydrogen bonds between the ammonium hydrogen and the amino nitrogen atom forming four distinct chains, each built up of three crystallographically independent enH+ cations. Two of these chains are running parallel to [100], the other two are parallel to [010]. Based on this arrangement different centrosymmetric or non-centrosymmetric hydrogen bonding patterns are possible, but only in one chain the sequence of NH2 and NH3 + groups was determined by X-ray diffraction