Solvothermal synthesis of novel antimony sulphides containing [Sb 4S7]2- units

Paz Vaqueiro; David P. Darlow; Anthony V. Powell; Ann M. Chippindale

doi:10.1016/j.ssi.2004.01.064

Solvothermal synthesis of novel antimony sulphides containing [Sb ₄S₇]^2- units

Paz Vaqueiro, David P. Darlow, Anthony V. Powell, Ann M. Chippindale

School of Engineering & Physical Sciences

Research output: Contribution to journal › Article › peer-review

82 Citations (Scopus)

Abstract

Two new antimony sulphides have been prepared solvothermally and characterised by single-crystal X-ray diffraction. [Co(en)₃][Sb ₄S₇] (1) was prepared at 140 °C from CoS, Sb ₂S₃ and S in the presence of ethylenediamine, whilst heating a mixture of Sb₂S₃, Co and S in tris(2-aminoethyl)amine, N(CH₂CH₂NH₂) ₃, at 180 °C results in the formation of [C₆H ₂₀N₄][Sb₄S₇] (2). Both materials contain [Sb₄S₇]^2- chains formed from linkage of cyclic Sb₃S₆^3- units by SbS₃^3- pyramids. In (1), the [Sb₄S₇]^2- chains are linked by secondary Sb-S interactions to form sheets, between which the charge balancing [Co(en)₃]²⁺ cations reside. The structure of (2) involves interconnection of pairs of [Sb₄S ₇]^2- chains through Sb₂S₂ rings to form isolated [Sb₄S₇]^2- double chains which are interleaved by protonated template molecules. © 2004 Elsevier B.V. All rights reserved.

Original language	English
Pages (from-to)	601-605
Number of pages	5
Journal	Solid State Ionics
Volume	172
Issue number	1-4 SPEC. ISS.
DOIs	https://doi.org/10.1016/j.ssi.2004.01.064
Publication status	Published - 31 Aug 2004

Keywords

Antimony sulphide
Crystal structure
Solvothermal synthesis

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10.1016/j.ssi.2004.01.064

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@article{1bc7c05154924d9391258aa7b2f3cb42,

title = "Solvothermal synthesis of novel antimony sulphides containing [Sb 4S7]2- units",

abstract = "Two new antimony sulphides have been prepared solvothermally and characterised by single-crystal X-ray diffraction. [Co(en)3][Sb 4S7] (1) was prepared at 140 °C from CoS, Sb 2S3 and S in the presence of ethylenediamine, whilst heating a mixture of Sb2S3, Co and S in tris(2-aminoethyl)amine, N(CH2CH2NH2) 3, at 180 °C results in the formation of [C6H 20N4][Sb4S7] (2). Both materials contain [Sb4S7]2- chains formed from linkage of cyclic Sb3S63- units by SbS33- pyramids. In (1), the [Sb4S7]2- chains are linked by secondary Sb-S interactions to form sheets, between which the charge balancing [Co(en)3]2+ cations reside. The structure of (2) involves interconnection of pairs of [Sb4S 7]2- chains through Sb2S2 rings to form isolated [Sb4S7]2- double chains which are interleaved by protonated template molecules. {\textcopyright} 2004 Elsevier B.V. All rights reserved.",

keywords = "Antimony sulphide, Crystal structure, Solvothermal synthesis",

author = "Paz Vaqueiro and Darlow, \{David P.\} and Powell, \{Anthony V.\} and Chippindale, \{Ann M.\}",

year = "2004",

month = aug,

day = "31",

doi = "10.1016/j.ssi.2004.01.064",

language = "English",

volume = "172",

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journal = "Solid State Ionics",

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number = "1-4 SPEC. ISS.",

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TY - JOUR

T1 - Solvothermal synthesis of novel antimony sulphides containing [Sb 4S7]2- units

AU - Vaqueiro, Paz

AU - Darlow, David P.

AU - Powell, Anthony V.

AU - Chippindale, Ann M.

PY - 2004/8/31

Y1 - 2004/8/31

N2 - Two new antimony sulphides have been prepared solvothermally and characterised by single-crystal X-ray diffraction. [Co(en)3][Sb 4S7] (1) was prepared at 140 °C from CoS, Sb 2S3 and S in the presence of ethylenediamine, whilst heating a mixture of Sb2S3, Co and S in tris(2-aminoethyl)amine, N(CH2CH2NH2) 3, at 180 °C results in the formation of [C6H 20N4][Sb4S7] (2). Both materials contain [Sb4S7]2- chains formed from linkage of cyclic Sb3S63- units by SbS33- pyramids. In (1), the [Sb4S7]2- chains are linked by secondary Sb-S interactions to form sheets, between which the charge balancing [Co(en)3]2+ cations reside. The structure of (2) involves interconnection of pairs of [Sb4S 7]2- chains through Sb2S2 rings to form isolated [Sb4S7]2- double chains which are interleaved by protonated template molecules. © 2004 Elsevier B.V. All rights reserved.

AB - Two new antimony sulphides have been prepared solvothermally and characterised by single-crystal X-ray diffraction. [Co(en)3][Sb 4S7] (1) was prepared at 140 °C from CoS, Sb 2S3 and S in the presence of ethylenediamine, whilst heating a mixture of Sb2S3, Co and S in tris(2-aminoethyl)amine, N(CH2CH2NH2) 3, at 180 °C results in the formation of [C6H 20N4][Sb4S7] (2). Both materials contain [Sb4S7]2- chains formed from linkage of cyclic Sb3S63- units by SbS33- pyramids. In (1), the [Sb4S7]2- chains are linked by secondary Sb-S interactions to form sheets, between which the charge balancing [Co(en)3]2+ cations reside. The structure of (2) involves interconnection of pairs of [Sb4S 7]2- chains through Sb2S2 rings to form isolated [Sb4S7]2- double chains which are interleaved by protonated template molecules. © 2004 Elsevier B.V. All rights reserved.

KW - Antimony sulphide

KW - Crystal structure

KW - Solvothermal synthesis

U2 - 10.1016/j.ssi.2004.01.064

DO - 10.1016/j.ssi.2004.01.064

M3 - Article

VL - 172

SP - 601

EP - 605

JO - Solid State Ionics

JF - Solid State Ionics

IS - 1-4 SPEC. ISS.