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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 : 000840 ( Istex/Corpus ); précédent : 000839; suivant : 000841

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

Auteurs : Michael Schaefer ; Lars Engelke ; Wolfgang Bensch

Source :

RBID : ISTEX:637949FA0E71F965F680DAB35125392C426BED64

English descriptors

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.

Url:
DOI: 10.1002/zaac.200300158

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ISTEX:637949FA0E71F965F680DAB35125392C426BED64

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<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>
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<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.</abstract>
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<title level="a" type="main">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>
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<title level="a" type="main">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>
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<forename type="first">Lars</forename>
<surname>Engelke</surname>
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<address>
<addrLine>Kiel</addrLine>
<addrLine>Institut für Anorganische Chemie der Christian‐Albrechts Universität</addrLine>
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<forename type="first">Wolfgang</forename>
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</persName>
<email>wbensch@ac.uni‐kiel.de</email>
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<abstract xml:lang="en" style="main">
<head>Abstract</head>
<p>The two novel thioantimonate(V) compounds [Mn(C
<hi rend="subscript">6</hi>
H
<hi rend="subscript">18</hi>
N
<hi rend="subscript">4</hi>
)(C
<hi rend="subscript">6</hi>
H
<hi rend="subscript">19</hi>
N
<hi rend="subscript">4</hi>
)]SbS
<hi rend="subscript">4</hi>
(
<hi rend="bold">I</hi>
) and [Mn(C
<hi rend="subscript">6</hi>
H
<hi rend="subscript">14</hi>
N
<hi rend="subscript">2</hi>
)
<hi rend="subscript">3</hi>
]
<formula>
<math>
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<mtext></mtext>
<mrow>
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[Mn(C
<hi rend="subscript">6</hi>
H
<hi rend="subscript">14</hi>
N
<hi rend="subscript">2</hi>
)
<hi rend="subscript">2</hi>
(SbS
<hi rend="subscript">4</hi>
)
<hi rend="subscript">2</hi>
]·6H
<hi rend="subscript">2</hi>
O (
<hi rend="bold">II</hi>
) 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 (
<hi rend="italic">trans</hi>
‐1, 2‐diaminocyclohexane, aqueous solution 50 %) at 130 °C. Compound
<hi rend="bold">I</hi>
crystallises in the triclinic space group
<hi rend="italic">P</hi>
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
<hi rend="superscript">3</hi>
, Z = 2, and
<hi rend="bold">II</hi>
in the monoclinic space group
<hi rend="italic">C</hi>
2/c, a = 32.611(2), b = 13.680(1), c = 19.997(1)Å, β = 117.237(5)°, V = 7931.7(8)Å
<hi rend="superscript">3</hi>
, Z = 4. In
<hi rend="bold">I</hi>
the Mn
<hi rend="superscript">2+</hi>
cation is surrounded by one tetradentate tren molecule, one protonated tren acting as a monodentate ligand and a monodentate [SbS
<hi rend="subscript">4</hi>
]
<hi rend="superscript">3—</hi>
anion yielding a distorted octahedral environment. In
<hi rend="bold">II</hi>
one unique Mn
<hi rend="superscript">2+</hi>
ion is in an octahedral environment of three bidentate chxn molecules and the second independent Mn
<hi rend="superscript">2+</hi>
ion is coordinated by two chxn ligands and two monodentate [SbS
<hi rend="subscript">4</hi>
]
<hi rend="superscript">3—</hi>
units leading to a distorted octahedral surrounding. The compounds were investigated and characterized with thermal and spectroscopic methods.</p>
</abstract>
<abstract xml:lang="de" style="main">
<p>
<hi rend="bold">Solvothermale Synthese und Kristallstrukturen zweier Thioantimonat(V)‐Verbindungen mit dem einzähnig wirkenden [SbS
<hi rend="subscript">4</hi>
]
<hi rend="superscript">3—</hi>
‐Anion: [Mn(C
<hi rend="subscript">6</hi>
H
<hi rend="subscript">18</hi>
N
<hi rend="subscript">4</hi>
)(C
<hi rend="subscript">6</hi>
H
<hi rend="subscript">19</hi>
N
<hi rend="subscript">4</hi>
)]SbS
<hi rend="subscript">4</hi>
und [Mn(C
<hi rend="subscript">6</hi>
H
<hi rend="subscript">14</hi>
N
<hi rend="subscript">2</hi>
)
<hi rend="subscript">3</hi>
]
<hi rend="subscript">2</hi>
[Mn(C
<hi rend="subscript">6</hi>
H
<hi rend="subscript">14</hi>
N
<hi rend="subscript">2</hi>
)
<hi rend="subscript">2</hi>
(SbS
<hi rend="subscript">4</hi>
)
<hi rend="subscript">2</hi>
]·6H
<hi rend="subscript">2</hi>
O</hi>
</p>
<p>Die beiden neuen Thioantimonate(V) [Mn(C
<hi rend="subscript">6</hi>
H
<hi rend="subscript">18</hi>
N
<hi rend="subscript">4</hi>
)(C
<hi rend="subscript">6</hi>
H
<hi rend="subscript">19</hi>
N
<hi rend="subscript">4</hi>
)]SbS
<hi rend="subscript">4</hi>
(
<hi rend="bold">I</hi>
) und [Mn(C
<hi rend="subscript">6</hi>
H
<hi rend="subscript">14</hi>
N
<hi rend="subscript">2</hi>
)
<hi rend="subscript">3</hi>
]
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</mrow>
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</formula>
[Mn(C
<hi rend="subscript">6</hi>
H
<hi rend="subscript">14</hi>
N
<hi rend="subscript">2</hi>
)
<hi rend="subscript">2</hi>
(SbS
<hi rend="subscript">4</hi>
)
<hi rend="subscript">2</hi>
]·6H
<hi rend="subscript">2</hi>
O (
<hi rend="bold">II</hi>
) 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 (
<hi rend="italic">trans</hi>
‐1, 2‐Diaminocyclohexan, 50 %‐ige Lösung) bei 130 °C gebildet. Verbindung
<hi rend="bold">I</hi>
kristallisiert in der triklinen Raumgruppe
<hi rend="italic">P</hi>
1¯, 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)Å
<hi rend="superscript">3</hi>
, Z = 2, und
<hi rend="bold">II</hi>
in der monoklinen Raumgruppe
<hi rend="italic">C</hi>
2/c, a = 32, 611(2)Å, b = 13, 680(1)Å, c = 19, 997(1)Å, β = 117, 237(5)°, V = 7931, 7(8)Å
<hi rend="superscript">3</hi>
, Z = 4. In
<hi rend="bold">I</hi>
ist das Mn
<hi rend="superscript">2+</hi>
‐Kation von einem vierzähnigen tren‐Liganden, einem einfach protonierten, einzähnigen tren‐Liganden sowie einem einzähnig wirkenden [SbS
<hi rend="subscript">4</hi>
]
<hi rend="superscript">3—</hi>
‐Anion verzerrt oktaedrisch umgeben. In
<hi rend="bold">II</hi>
befindet sich ein unabhängiges Mn
<hi rend="superscript">2+</hi>
‐Ion in einer oktaedrischen Umgebung aus drei zweizähnigen chxn‐Liganden, das zweite unabhängige Mn
<hi rend="superscript">2+</hi>
‐Ion ist verzerrt oktaedrisch von zwei chxn‐Liganden sowie zwei einzähnigen [SbS
<hi rend="subscript">4</hi>
]
<hi rend="superscript">3—</hi>
‐Einheiten koordiniert. Die Verbindungen wurden mit thermischen und spektroskopischen Methoden untersucht und charakterisiert.</p>
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<title type="main" xml:lang="en">Solvothermal Synthesis and Crystal Structures of Two Thioantimonate(V) Compounds with the [SbS
<sub>4</sub>
]
<sup>3—</sup>
Anion Acting as a Monodentate Ligand: [Mn(C
<sub>6</sub>
H
<sub>18</sub>
N
<sub>4</sub>
)(C
<sub>6</sub>
H
<sub>19</sub>
N
<sub>4</sub>
)]SbS
<sub>4</sub>
and [Mn(C
<sub>6</sub>
H
<sub>14</sub>
N
<sub>2</sub>
)
<sub>3</sub>
]
<sub>2</sub>
[Mn(C
<sub>6</sub>
H
<sub>14</sub>
N
<sub>2</sub>
)
<sub>2</sub>
(SbS
<sub>4</sub>
)
<sub>2</sub>
]·6H
<sub>2</sub>
O</title>
</titleGroup>
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<personName>
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</personName>
</creator>
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<personName>
<givenNames>Lars</givenNames>
<familyName>Engelke</familyName>
</personName>
</creator>
<creator xml:id="au3" creatorRole="author" affiliationRef="#a1" corresponding="yes">
<personName>
<givenNames>Wolfgang</givenNames>
<familyName>Bensch</familyName>
<degrees>Prof. Dr.</degrees>
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<keyword xml:id="kwd1">Thioantimonate</keyword>
<keyword xml:id="kwd2">Solvothermal synthesis</keyword>
<keyword xml:id="kwd3">Thermal stability</keyword>
<keyword xml:id="kwd4">Raman spectroscopy</keyword>
</keywordGroup>
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<abstract type="main" xml:lang="en">
<title type="main">Abstract</title>
<p>The two novel thioantimonate(V) compounds [Mn(C
<sub>6</sub>
H
<sub>18</sub>
N
<sub>4</sub>
)(C
<sub>6</sub>
H
<sub>19</sub>
N
<sub>4</sub>
)]SbS
<sub>4</sub>
(
<b>I</b>
) and [Mn(C
<sub>6</sub>
H
<sub>14</sub>
N
<sub>2</sub>
)
<sub>3</sub>
]
<math altimg="urn:x-wiley:00442313:media:ZAAC200300158:tex2gif-inf-32" wiley:location="equation/tex2gif-inf-32.gif">
<msub>
<mtext></mtext>
<mrow>
<msup>
<mtext></mtext>
<mrow>
<mtext>2—</mtext>
</mrow>
</msup>
</mrow>
</msub>
</math>
[Mn(C
<sub>6</sub>
H
<sub>14</sub>
N
<sub>2</sub>
)
<sub>2</sub>
(SbS
<sub>4</sub>
)
<sub>2</sub>
]·6H
<sub>2</sub>
O (
<b>II</b>
) 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 (
<i>trans</i>
‐1, 2‐diaminocyclohexane, aqueous solution 50 %) at 130 °C. Compound
<b>I</b>
crystallises in the triclinic space group
<i>P</i>
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
<sup>3</sup>
, Z = 2, and
<b>II</b>
in the monoclinic space group
<i>C</i>
2/c, a = 32.611(2), b = 13.680(1), c = 19.997(1)Å, β = 117.237(5)°, V = 7931.7(8)Å
<sup>3</sup>
, Z = 4. In
<b>I</b>
the Mn
<sup>2+</sup>
cation is surrounded by one tetradentate tren molecule, one protonated tren acting as a monodentate ligand and a monodentate [SbS
<sub>4</sub>
]
<sup>3—</sup>
anion yielding a distorted octahedral environment. In
<b>II</b>
one unique Mn
<sup>2+</sup>
ion is in an octahedral environment of three bidentate chxn molecules and the second independent Mn
<sup>2+</sup>
ion is coordinated by two chxn ligands and two monodentate [SbS
<sub>4</sub>
]
<sup>3—</sup>
units leading to a distorted octahedral surrounding. The compounds were investigated and characterized with thermal and spectroscopic methods.</p>
</abstract>
<abstract type="main" xml:lang="de">
<p>
<b>Solvothermale Synthese und Kristallstrukturen zweier Thioantimonat(V)‐Verbindungen mit dem einzähnig wirkenden [SbS
<sub>4</sub>
]
<sup>3—</sup>
‐Anion: [Mn(C
<sub>6</sub>
H
<sub>18</sub>
N
<sub>4</sub>
)(C
<sub>6</sub>
H
<sub>19</sub>
N
<sub>4</sub>
)]SbS
<sub>4</sub>
und [Mn(C
<sub>6</sub>
H
<sub>14</sub>
N
<sub>2</sub>
)
<sub>3</sub>
]
<sub>2</sub>
[Mn(C
<sub>6</sub>
H
<sub>14</sub>
N
<sub>2</sub>
)
<sub>2</sub>
(SbS
<sub>4</sub>
)
<sub>2</sub>
]·6H
<sub>2</sub>
O</b>
</p>
<p>Die beiden neuen Thioantimonate(V) [Mn(C
<sub>6</sub>
H
<sub>18</sub>
N
<sub>4</sub>
)(C
<sub>6</sub>
H
<sub>19</sub>
N
<sub>4</sub>
)]SbS
<sub>4</sub>
(
<b>I</b>
) und [Mn(C
<sub>6</sub>
H
<sub>14</sub>
N
<sub>2</sub>
)
<sub>3</sub>
]
<math altimg="urn:x-wiley:00442313:media:ZAAC200300158:tex2gif-inf-73" wiley:location="equation/tex2gif-inf-73.gif">
<msub>
<mtext></mtext>
<mrow>
<mtext>2</mtext>
<msup>
<mtext></mtext>
<mrow>
<mtext></mtext>
</mrow>
</msup>
</mrow>
</msub>
</math>
[Mn(C
<sub>6</sub>
H
<sub>14</sub>
N
<sub>2</sub>
)
<sub>2</sub>
(SbS
<sub>4</sub>
)
<sub>2</sub>
]·6H
<sub>2</sub>
O (
<b>II</b>
) 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 (
<i>trans</i>
‐1, 2‐Diaminocyclohexan, 50 %‐ige Lösung) bei 130 °C gebildet. Verbindung
<b>I</b>
kristallisiert in der triklinen Raumgruppe
<i>P</i>
1¯, 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)Å
<sup>3</sup>
, Z = 2, und
<b>II</b>
in der monoklinen Raumgruppe
<i>C</i>
2/c, a = 32, 611(2)Å, b = 13, 680(1)Å, c = 19, 997(1)Å, β = 117, 237(5)°, V = 7931, 7(8)Å
<sup>3</sup>
, Z = 4. In
<b>I</b>
ist das Mn
<sup>2+</sup>
‐Kation von einem vierzähnigen tren‐Liganden, einem einfach protonierten, einzähnigen tren‐Liganden sowie einem einzähnig wirkenden [SbS
<sub>4</sub>
]
<sup>3—</sup>
‐Anion verzerrt oktaedrisch umgeben. In
<b>II</b>
befindet sich ein unabhängiges Mn
<sup>2+</sup>
‐Ion in einer oktaedrischen Umgebung aus drei zweizähnigen chxn‐Liganden, das zweite unabhängige Mn
<sup>2+</sup>
‐Ion ist verzerrt oktaedrisch von zwei chxn‐Liganden sowie zwei einzähnigen [SbS
<sub>4</sub>
]
<sup>3—</sup>
‐Einheiten koordiniert. Die Verbindungen wurden mit thermischen und spektroskopischen Methoden untersucht und charakterisiert.</p>
</abstract>
</abstractGroup>
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<titleInfo lang="en">
<title>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>
</titleInfo>
<titleInfo type="alternative" contentType="CDATA" lang="en">
<title>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>
</titleInfo>
<name type="personal">
<namePart type="given">Michael</namePart>
<namePart type="family">Schaefer</namePart>
<affiliation>Kiel, Institut für Anorganische Chemie der Christian‐Albrechts Universität</affiliation>
<role>
<roleTerm type="text">author</roleTerm>
</role>
</name>
<name type="personal">
<namePart type="given">Lars</namePart>
<namePart type="family">Engelke</namePart>
<affiliation>Kiel, Institut für Anorganische Chemie der Christian‐Albrechts Universität</affiliation>
<role>
<roleTerm type="text">author</roleTerm>
</role>
</name>
<name type="personal">
<namePart type="given">Wolfgang</namePart>
<namePart type="family">Bensch</namePart>
<namePart type="termsOfAddress">Prof. Dr.</namePart>
<affiliation>Kiel, Institut für Anorganische Chemie der Christian‐Albrechts Universität</affiliation>
<affiliation>E-mail: wbensch@ac.uni‐kiel.de</affiliation>
<affiliation>Correspondence address: Institut für Anorganische Chemie der Universität Kiel, Olshausenstr. 40, D‐24098 Kiel, Fax: +49 (0)431/880 — 1520</affiliation>
<role>
<roleTerm type="text">author</roleTerm>
</role>
</name>
<typeOfResource>text</typeOfResource>
<genre type="article" displayLabel="article" authority="ISTEX" authorityURI="https://content-type.data.istex.fr" valueURI="https://content-type.data.istex.fr/ark:/67375/XTP-6N5SZHKN-D">article</genre>
<originInfo>
<publisher>WILEY‐VCH Verlag</publisher>
<place>
<placeTerm type="text">Weinheim</placeTerm>
</place>
<dateIssued encoding="w3cdtf">2003-10</dateIssued>
<dateCaptured encoding="w3cdtf">2003-05-09</dateCaptured>
<copyrightDate encoding="w3cdtf">2003</copyrightDate>
</originInfo>
<language>
<languageTerm type="code" authority="rfc3066">en</languageTerm>
<languageTerm type="code" authority="iso639-2b">eng</languageTerm>
</language>
<physicalDescription>
<extent unit="figures">8</extent>
<extent unit="tables">5</extent>
<extent unit="references">22</extent>
</physicalDescription>
<abstract 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.</abstract>
<abstract 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.</abstract>
<subject lang="en">
<genre>keywords</genre>
<topic>Thioantimonate</topic>
<topic>Solvothermal synthesis</topic>
<topic>Thermal stability</topic>
<topic>Raman spectroscopy</topic>
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