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New Thioantimonates(III) with Different Sb:S Ratios: Solvothermal Syntheses and Crystal Structures of [(C3H10NO)(C3H10N)][Sb8S13], [(C2H8NO)(C2H8N)(CH5N)][Sb8S13], [(C6H16N2)(C6H14N2)][Sb6S10], and [C8H22N2][Sb4S7]

Identifieur interne : 000D27 ( Main/Exploration ); précédent : 000D26; suivant : 000D28

New Thioantimonates(III) with Different Sb:S Ratios: Solvothermal Syntheses and Crystal Structures of [(C3H10NO)(C3H10N)][Sb8S13], [(C2H8NO)(C2H8N)(CH5N)][Sb8S13], [(C6H16N2)(C6H14N2)][Sb6S10], and [C8H22N2][Sb4S7]

Auteurs : Beatrix Seidlhofer [Allemagne] ; Volker Spetzler [Allemagne] ; Enrique Quiroga-Gonzalez [Allemagne] ; Christian N Ther [Allemagne] ; Wolfgang Bensch [Allemagne]

Source :

RBID : ISTEX:F04FD26B1D3DD73E4B488C5BE5D755AA051F6E2E

English descriptors

Abstract

Four new thioantimonates(III) with compositions [(C3H10NO)(C3H10N)][Sb8S13] (1) (C3H9NO = 1‐amino‐3‐propanol, C3H9N = propylamine), [(C2H8NO)(C2H8N)(CH5N)][Sb8S13] (2) (C2H7NO = ethanolamine, C2H7N = ethylamine, CH5N = methylamine), [(C6H16N2)(C6H14N2)][Sb6S10] (3) (C6H14N2 = 1,2‐diaminocyclohexane) and [C8H22N2][Sb4S7] (4) (C8H20N2 = 1,8‐diaminooctane) were synthesized under solvothermal conditions. Compound 1: triclinic space group P$\bar{1}$, a = 6.9695(6) Å, b = 13.8095(12) Å, c = 18.0354(17) Å, α = 98.367(11), β = 96.097(11) and γ = 101.281(11)°; compound 2: monoclinic space group P21/m, a = 7.1668(5), b = 25.8986(14), c = 16.0436(11) Å, β = 96.847(8)°; compound 3: monoclinic space group P21/n, a = 11.6194(9), b = 10.2445(5) Å, c = 27.3590(18) Å, β = 91.909(6)°; compound 4: triclinic space group P$\bar{1}$, a = 7.0743(6), b = 12.0846(11), c = 13.9933(14) Å, α = 114.723(10), β = 97.595(11), γ = 93.272(11)°. The main structural feature of the two atoms thick layered [Sb8S13]2– anion in 1 are large nearly rectangular pores with dimensions 11.2 × 11.7 Å. The layers are stacked perpendicular to [100] to form tunnels being directed along [100]. In contrast to 1 the structure of 2 contains a [Sb8S13]2– chain anion with Sb12S12 pores measuring about 8.9 × 11.5 Å. Only if longer Sb–S distances are considered as bonding interactions a layered anion is formed. The chain anion [Sb6S10]2– in compound 3 is unique and is constructed by corner‐sharing SbS3 pyramids. Two symmetry‐related single chains consisting of alternating SbS3 units and Sb3S3 rings are bound to Sb4S4 rings in chair conformation. Finally, in the structure of 4 the SbS3 and SbS4 moieties are joined corner‐linked to form a chain of alternating SbS4 units and (SbS3)3 blocks. Neighboring chains are connected into sheets that contain relatively large Sb10S10 heterorings. The sheets are further connected by sulfur atoms generating four atoms thick double sheets.

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DOI: 10.1002/zaac.201100204


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<title xml:lang="en">New Thioantimonates(III) with Different Sb:S Ratios: Solvothermal Syntheses and Crystal Structures of [(C3H10NO)(C3H10N)][Sb8S13], [(C2H8NO)(C2H8N)(CH5N)][Sb8S13], [(C6H16N2)(C6H14N2)][Sb6S10], and [C8H22N2][Sb4S7]</title>
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<name sortKey="Seidlhofer, Beatrix" sort="Seidlhofer, Beatrix" uniqKey="Seidlhofer B" first="Beatrix" last="Seidlhofer">Beatrix Seidlhofer</name>
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<name sortKey="Quiroga Onzalez, Enrique" sort="Quiroga Onzalez, Enrique" uniqKey="Quiroga Onzalez E" first="Enrique" last="Quiroga-Gonzalez">Enrique Quiroga-Gonzalez</name>
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<term>Acta crystallogr</term>
<term>Allg</term>
<term>Amine</term>
<term>Amine molecules</term>
<term>Amino alcohols</term>
<term>Anion</term>
<term>Anorg</term>
<term>Antimony</term>
<term>Antimony atoms</term>
<term>Bensch</term>
<term>Bensch table</term>
<term>Bond lengths</term>
<term>Chain anion</term>
<term>Chair conformation</term>
<term>Chem</term>
<term>Chippindale</term>
<term>Crystal structures</term>
<term>Equivalent atoms</term>
<term>Ethanolamine</term>
<term>Gmbh</term>
<term>Hydrogen atoms</term>
<term>Inorg</term>
<term>Kgaa</term>
<term>Mmol</term>
<term>Moiety</term>
<term>Molecule</term>
<term>Monoclinic space group</term>
<term>Naturforsch</term>
<term>Pyramid</term>
<term>Sbs3</term>
<term>Sbs3 pyramids</term>
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<term>Solid state chem</term>
<term>Solvothermal</term>
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<term>Solvothermal syntheses</term>
<term>Space group</term>
<term>Spetzler</term>
<term>Sulfur</term>
<term>Sulfur atoms</term>
<term>Symmetry transformations</term>
<term>Thioantimonates</term>
<term>Topology</term>
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<div type="abstract" xml:lang="en">Four new thioantimonates(III) with compositions [(C3H10NO)(C3H10N)][Sb8S13] (1) (C3H9NO = 1‐amino‐3‐propanol, C3H9N = propylamine), [(C2H8NO)(C2H8N)(CH5N)][Sb8S13] (2) (C2H7NO = ethanolamine, C2H7N = ethylamine, CH5N = methylamine), [(C6H16N2)(C6H14N2)][Sb6S10] (3) (C6H14N2 = 1,2‐diaminocyclohexane) and [C8H22N2][Sb4S7] (4) (C8H20N2 = 1,8‐diaminooctane) were synthesized under solvothermal conditions. Compound 1: triclinic space group P$\bar{1}$, a = 6.9695(6) Å, b = 13.8095(12) Å, c = 18.0354(17) Å, α = 98.367(11), β = 96.097(11) and γ = 101.281(11)°; compound 2: monoclinic space group P21/m, a = 7.1668(5), b = 25.8986(14), c = 16.0436(11) Å, β = 96.847(8)°; compound 3: monoclinic space group P21/n, a = 11.6194(9), b = 10.2445(5) Å, c = 27.3590(18) Å, β = 91.909(6)°; compound 4: triclinic space group P$\bar{1}$, a = 7.0743(6), b = 12.0846(11), c = 13.9933(14) Å, α = 114.723(10), β = 97.595(11), γ = 93.272(11)°. The main structural feature of the two atoms thick layered [Sb8S13]2– anion in 1 are large nearly rectangular pores with dimensions 11.2 × 11.7 Å. The layers are stacked perpendicular to [100] to form tunnels being directed along [100]. In contrast to 1 the structure of 2 contains a [Sb8S13]2– chain anion with Sb12S12 pores measuring about 8.9 × 11.5 Å. Only if longer Sb–S distances are considered as bonding interactions a layered anion is formed. The chain anion [Sb6S10]2– in compound 3 is unique and is constructed by corner‐sharing SbS3 pyramids. Two symmetry‐related single chains consisting of alternating SbS3 units and Sb3S3 rings are bound to Sb4S4 rings in chair conformation. Finally, in the structure of 4 the SbS3 and SbS4 moieties are joined corner‐linked to form a chain of alternating SbS4 units and (SbS3)3 blocks. Neighboring chains are connected into sheets that contain relatively large Sb10S10 heterorings. The sheets are further connected by sulfur atoms generating four atoms thick double sheets.</div>
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<name sortKey="Bensch, Wolfgang" sort="Bensch, Wolfgang" uniqKey="Bensch W" first="Wolfgang" last="Bensch">Wolfgang Bensch</name>
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