Synthesis and Structure of [CH3NH3]2Sb8S13: A Nanoporous Thioantimonate(III) with a Two-Dimensional Channel System

✍ Scribed by Xiqu Wang; Friedrich Liebau

• Publisher: Elsevier Science
• Year: 1994
• Tongue: English
• Weight: 229 KB
• Volume: 111
• Category: Article
• ISSN: 0022-4596
• DOI: 10.1006/jssc.1994.1243

✦ Synopsis

(\left[\mathrm{CH}{3} \mathrm{NH}{3}\right]{2} \mathrm{Sb}{8} \mathrm{~S}{13}) has been synthesized as dark-red plate-like crystals by heating (\mathrm{Sb}) and (\mathrm{S}) with an aqueous solution of (\mathrm{CH}{3} \mathrm{NH}{2}) between 130 and (190^{\circ} \mathrm{C}). It is triclinic, space group (P{\overline{1}}), with (a=15.866(3) \AA, b=11.581(2) \AA, c=8.295(2) \AA, \alpha=71.46(2)^{\circ}), (\beta=75.71(2)^{\circ}, \gamma=82.25(2)^{\circ}), and (Z=2). The structure was determined and refined with 3342 independent single crystal Xray reflections (235 parameters, (R=0.061, R_{\mathrm{w}}=0.052) ). Each (\mathrm{Sb}) atom forms three short bonds to (S) reflecting the influence of a lone electron pair. Of the eight nonequivalent (\mathrm{Sb}) atoms, three have one longer bond and four other (\mathrm{Sb}) atoms have two longer bonds to (\mathrm{S}). The (\left[\mathrm{SbS}{n}\right]) polyhedra share corners and edges to form a three-dimensional framework. This framework is traversed by a system of two types of intersecting channels parallel to [010] and [001]. (\left[\mathrm{CH}{3} \mathrm{NH}_{3}\right]^{+})cations located in the channel intersections are orientationally disordered; those in pockets of the [010] channels are ordered. O 1994 Academic Press, Inc.