Solvothermal Synthesis and Crystal Structures of Two Thioantimonate(V) Compounds with the [SbS4]3— Anion Acting as a Monodentate Ligand: [Mn(C6H18N4)(C6H19N4)]SbS4 and [Mn(C6H14N2)3]2[Mn(C6H14N2)2(SbS4)2]·6H2O
Identifieur interne : 001716 ( Main/Exploration ); précédent : 001715; suivant : 001717Solvothermal Synthesis and Crystal Structures of Two Thioantimonate(V) Compounds with the [SbS4]3— Anion Acting as a Monodentate Ligand: [Mn(C6H18N4)(C6H19N4)]SbS4 and [Mn(C6H14N2)3]2[Mn(C6H14N2)2(SbS4)2]·6H2O
Auteurs : Michael Schaefer ; Lars Engelke ; Wolfgang Bensch [Allemagne]Source :
- ZAAC ‐ Journal of Inorganic and General Chemistry [ 0044-2313 ] ; 2003-10.
English descriptors
- Teeft :
- Acta crystallogr, Allg, Amine, Amine molecules, Angles range, Anion, Anorg, Atomic coordinates, Bensch, Bensch table, Bond lengths, Cation, Chem, Chxn, Chxn ligands, Crystal structure, Crystal structures, Different steps, Disordered atoms, Experimental value, Final occupancies, General positions, Gmbh, Heating rate, Hydrogen atoms, Hydrogen bonds, Inner volume, Isotropic displacement, Kgaa, Ligand, Monodentate, Monodentate ligand, Octahedral environment, Powder pattern, Raman, Raman spectra, Room temperature, Sbs4 tetrahedra, Solvothermal synthesis, Split positions, Standard deviations, Steel autoclave, Sterical demand, Thermal decomposition, Thermal stability, Tren, Verlag, Verlag gmbh, Water molecules, Weight loss, Weinheim.
Abstract
The two novel thioantimonate(V) compounds [Mn(C6H18N4)(C6H19N4)]SbS4 (I) and [Mn(C6H14N2)3] 2—[Mn(C6H14N2)2(SbS4)2]·6H2O (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 P1¯, 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)Å3, Z = 2, and II in the monoclinic space group C2/c, a = 32.611(2), b = 13.680(1), c = 19.997(1)Å, β = 117.237(5)°, V = 7931.7(8)Å3, Z = 4. In I the Mn2+ cation is surrounded by one tetradentate tren molecule, one protonated tren acting as a monodentate ligand and a monodentate [SbS4]3— anion yielding a distorted octahedral environment. In II one unique Mn2+ ion is in an octahedral environment of three bidentate chxn molecules and the second independent Mn2+ ion is coordinated by two chxn ligands and two monodentate [SbS4]3— units leading to a distorted octahedral surrounding. The compounds were investigated and characterized with thermal and spectroscopic methods.
Solvothermale Synthese und Kristallstrukturen zweier Thioantimonat(V)‐Verbindungen mit dem einzähnig wirkenden [SbS4]3—‐Anion: [Mn(C6H18N4)(C6H19N4)]SbS4 und [Mn(C6H14N2)3]2[Mn(C6H14N2)2(SbS4)2]·6H2O Die beiden neuen Thioantimonate(V) [Mn(C6H18N4)(C6H19N4)]SbS4 (I) und [Mn(C6H14N2)3] 2 —[Mn(C6H14N2)2(SbS4)2]·6H2O (II) werden unter solvothermalen Bedingungen bei der Reaktion von Mangan, Antimon und Schwefel im stöchiometrischen Verhältnis in 5 ml Tris(2‐Aminoethyl)amin (tren) bei 140 °C oder chxn (trans‐1, 2‐Diaminocyclohexan, 50 %‐ige Lösung) bei 130 °C gebildet. Verbindung I kristallisiert in der triklinen Raumgruppe P1¯, a = 9, 578(2)Å, b = 11, 541(2)Å, c = 12, 297(2)Å, α = 62, 55(1)°, β = 85, 75(1)°, γ = 89, 44(1)°, V = 1202, 6(4)Å3, Z = 2, und II in der monoklinen Raumgruppe C2/c, a = 32, 611(2)Å, b = 13, 680(1)Å, c = 19, 997(1)Å, β = 117, 237(5)°, V = 7931, 7(8)Å3, Z = 4. In I ist das Mn2+‐Kation von einem vierzähnigen tren‐Liganden, einem einfach protonierten, einzähnigen tren‐Liganden sowie einem einzähnig wirkenden [SbS4]3—‐Anion verzerrt oktaedrisch umgeben. In II befindet sich ein unabhängiges Mn2+‐Ion in einer oktaedrischen Umgebung aus drei zweizähnigen chxn‐Liganden, das zweite unabhängige Mn2+‐Ion ist verzerrt oktaedrisch von zwei chxn‐Liganden sowie zwei einzähnigen [SbS4]3—‐Einheiten koordiniert. Die Verbindungen wurden mit thermischen und spektroskopischen Methoden untersucht und charakterisiert.
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DOI: 10.1002/zaac.200300158
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<record><TEI wicri:istexFullTextTei="biblStruct"><teiHeader><fileDesc><titleStmt><title xml:lang="en">Solvothermal Synthesis and Crystal Structures of Two Thioantimonate(V) Compounds with the [SbS4]3— Anion Acting as a Monodentate Ligand: [Mn(C6H18N4)(C6H19N4)]SbS4 and [Mn(C6H14N2)3]2[Mn(C6H14N2)2(SbS4)2]·6H2O</title><author><name sortKey="Schaefer, Michael" sort="Schaefer, Michael" uniqKey="Schaefer M" first="Michael" last="Schaefer">Michael Schaefer</name></author><author><name sortKey="Engelke, Lars" sort="Engelke, Lars" uniqKey="Engelke L" first="Lars" last="Engelke">Lars Engelke</name></author><author><name sortKey="Bensch, Wolfgang" sort="Bensch, Wolfgang" uniqKey="Bensch W" first="Wolfgang" last="Bensch">Wolfgang Bensch</name></author></titleStmt><publicationStmt><idno type="wicri:source">ISTEX</idno><idno type="RBID">ISTEX:637949FA0E71F965F680DAB35125392C426BED64</idno><date when="2003" year="2003">2003</date><idno type="doi">10.1002/zaac.200300158</idno><idno 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Michael" sort="Schaefer, Michael" uniqKey="Schaefer M" first="Michael" last="Schaefer">Michael Schaefer</name><affiliation><wicri:noCountry code="subField">Universität</wicri:noCountry></affiliation></author><author><name sortKey="Engelke, Lars" sort="Engelke, Lars" uniqKey="Engelke L" first="Lars" last="Engelke">Lars Engelke</name><affiliation><wicri:noCountry code="subField">Universität</wicri:noCountry></affiliation></author><author><name sortKey="Bensch, Wolfgang" sort="Bensch, Wolfgang" uniqKey="Bensch W" first="Wolfgang" last="Bensch">Wolfgang Bensch</name><affiliation></affiliation><affiliation wicri:level="1"><country wicri:rule="url">Allemagne</country></affiliation><affiliation></affiliation></author></analytic><monogr></monogr><series><title level="j" type="main">ZAAC ‐ Journal of Inorganic and General Chemistry</title><idno type="ISSN">0044-2313</idno><idno type="eISSN">1521-3749</idno><imprint><biblScope unit="vol">629</biblScope><biblScope unit="issue">11</biblScope><biblScope unit="page" from="1912">1912</biblScope><biblScope unit="page" to="1918">1918</biblScope><biblScope unit="page-count">7</biblScope><publisher>WILEY‐VCH Verlag</publisher><pubPlace>Weinheim</pubPlace><date type="published" when="2003-10">2003-10</date></imprint><idno type="ISSN">0044-2313</idno></series></biblStruct></sourceDesc><seriesStmt><idno type="ISSN">0044-2313</idno></seriesStmt></fileDesc><profileDesc><textClass><keywords scheme="Teeft" xml:lang="en"><term>Acta crystallogr</term><term>Allg</term><term>Amine</term><term>Amine molecules</term><term>Angles range</term><term>Anion</term><term>Anorg</term><term>Atomic coordinates</term><term>Bensch</term><term>Bensch table</term><term>Bond lengths</term><term>Cation</term><term>Chem</term><term>Chxn</term><term>Chxn ligands</term><term>Crystal structure</term><term>Crystal structures</term><term>Different steps</term><term>Disordered atoms</term><term>Experimental value</term><term>Final occupancies</term><term>General positions</term><term>Gmbh</term><term>Heating rate</term><term>Hydrogen atoms</term><term>Hydrogen bonds</term><term>Inner volume</term><term>Isotropic displacement</term><term>Kgaa</term><term>Ligand</term><term>Monodentate</term><term>Monodentate ligand</term><term>Octahedral environment</term><term>Powder pattern</term><term>Raman</term><term>Raman spectra</term><term>Room temperature</term><term>Sbs4 tetrahedra</term><term>Solvothermal synthesis</term><term>Split positions</term><term>Standard deviations</term><term>Steel autoclave</term><term>Sterical demand</term><term>Thermal decomposition</term><term>Thermal stability</term><term>Tren</term><term>Verlag</term><term>Verlag gmbh</term><term>Water molecules</term><term>Weight loss</term><term>Weinheim</term></keywords></textClass></profileDesc></teiHeader><front><div type="abstract" xml:lang="en">The two novel thioantimonate(V) compounds [Mn(C6H18N4)(C6H19N4)]SbS4 (I) and [Mn(C6H14N2)3] 2—[Mn(C6H14N2)2(SbS4)2]·6H2O (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 P1¯, 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)Å3, Z = 2, and II in the monoclinic space group C2/c, a = 32.611(2), b = 13.680(1), c = 19.997(1)Å, β = 117.237(5)°, V = 7931.7(8)Å3, Z = 4. In I the Mn2+ cation is surrounded by one tetradentate tren molecule, one protonated tren acting as a monodentate ligand and a monodentate [SbS4]3— anion yielding a distorted octahedral environment. In II one unique Mn2+ ion is in an octahedral environment of three bidentate chxn molecules and the second independent Mn2+ ion is coordinated by two chxn ligands and two monodentate [SbS4]3— units leading to a distorted octahedral surrounding. The compounds were investigated and characterized with thermal and spectroscopic methods.</div><div type="abstract" xml:lang="de">Solvothermale Synthese und Kristallstrukturen zweier Thioantimonat(V)‐Verbindungen mit dem einzähnig wirkenden [SbS4]3—‐Anion: [Mn(C6H18N4)(C6H19N4)]SbS4 und [Mn(C6H14N2)3]2[Mn(C6H14N2)2(SbS4)2]·6H2O Die beiden neuen Thioantimonate(V) [Mn(C6H18N4)(C6H19N4)]SbS4 (I) und [Mn(C6H14N2)3] 2 —[Mn(C6H14N2)2(SbS4)2]·6H2O (II) werden unter solvothermalen Bedingungen bei der Reaktion von Mangan, Antimon und Schwefel im stöchiometrischen Verhältnis in 5 ml Tris(2‐Aminoethyl)amin (tren) bei 140 °C oder chxn (trans‐1, 2‐Diaminocyclohexan, 50 %‐ige Lösung) bei 130 °C gebildet. Verbindung I kristallisiert in der triklinen Raumgruppe P1¯, a = 9, 578(2)Å, b = 11, 541(2)Å, c = 12, 297(2)Å, α = 62, 55(1)°, β = 85, 75(1)°, γ = 89, 44(1)°, V = 1202, 6(4)Å3, Z = 2, und II in der monoklinen Raumgruppe C2/c, a = 32, 611(2)Å, b = 13, 680(1)Å, c = 19, 997(1)Å, β = 117, 237(5)°, V = 7931, 7(8)Å3, Z = 4. In I ist das Mn2+‐Kation von einem vierzähnigen tren‐Liganden, einem einfach protonierten, einzähnigen tren‐Liganden sowie einem einzähnig wirkenden [SbS4]3—‐Anion verzerrt oktaedrisch umgeben. In II befindet sich ein unabhängiges Mn2+‐Ion in einer oktaedrischen Umgebung aus drei zweizähnigen chxn‐Liganden, das zweite unabhängige Mn2+‐Ion ist verzerrt oktaedrisch von zwei chxn‐Liganden sowie zwei einzähnigen [SbS4]3—‐Einheiten koordiniert. Die Verbindungen wurden mit thermischen und spektroskopischen Methoden untersucht und charakterisiert.</div></front></TEI><affiliations><list><country><li>Allemagne</li></country></list><tree><noCountry><name sortKey="Engelke, Lars" sort="Engelke, Lars" uniqKey="Engelke L" first="Lars" last="Engelke">Lars Engelke</name><name sortKey="Schaefer, Michael" sort="Schaefer, Michael" uniqKey="Schaefer M" first="Michael" last="Schaefer">Michael Schaefer</name></noCountry><country name="Allemagne"><noRegion><name sortKey="Bensch, Wolfgang" sort="Bensch, Wolfgang" uniqKey="Bensch W" first="Wolfgang" last="Bensch">Wolfgang Bensch</name></noRegion></country></tree></affiliations></record>Pour manipuler ce document sous Unix (Dilib)
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