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].

Seidlhofer, Beatrix, Spetzler, Volker, Quiroga-Gonzalez, Enrique, Näther, Christian and Bensch, Wolfgang (2011) 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]. Zeitschrift für anorganische und allgemeine Chemie, 637 (10). pp. 1295-1303. DOI 10.1002/zaac.201100204.

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Supplementary data:

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, 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, 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.

Document Type: Article
Research affiliation: Kiel University
Kiel University > Kiel Marine Science
OceanRep > The Future Ocean - Cluster of Excellence
Refereed: Yes
Open Access Journal?: No
Publisher: American Medical Association
Projects: Future Ocean
Date Deposited: 12 Jun 2018 10:51
Last Modified: 23 Sep 2019 23:07
URI: https://oceanrep.geomar.de/id/eprint/43345

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