Synthesis, electronic and crystal structures, and physical studies of the superconductor Cs(~1)Mo12S14, final step of the condensation of the Mo6L8(i)L6(a) unit

Patrick Gougeon; Diala Salloum; Jérôme Cuny; Laurent Le Pollès; Marie Le Floch; Régis Gautier; Michel Potel

doi:10.1021/ic900960g

Synthesis, electronic and crystal structures, and physical studies of the superconductor Cs(~1)Mo12S14, final step of the condensation of the Mo6L8(i)L6(a) unit

Inorg Chem. 2009 Sep 7;48(17):8337-41. doi: 10.1021/ic900960g.

Authors

Patrick Gougeon¹, Diala Salloum, Jérôme Cuny, Laurent Le Pollès, Marie Le Floch, Régis Gautier, Michel Potel

Affiliation

¹ Sciences Chimiques de Rennes, UMR CNRS 6226, Université de Rennes 1, Ecole Nationale Supérieure de Chimie de Rennes, 35042 Rennes Cedex, France. patrick.gougeon@univ-rennes1.fr

PMID: 19645498
DOI: 10.1021/ic900960g

Abstract

The ternary reduced molybdenum sulphide Cs(~1)Mo12S14 has been synthesized by solid-state reaction at 1400 degrees C for 96 h in sealed molybdenum crucibles. The compound crystallizes in the trigonal space group P31c with the following lattice parameters: a = 9.9793 (2) A, c = 6.3730 (2) A, Z = 1. Its crystal structure was determined from single crystal X-ray diffraction data and consists of interconnected Mo6S8(i)S6(a) units forming an original three-dimensional framework in which large tunnels are occupied randomly by the Cs+ ions. 133Cs static NMR studies are in favor of a static cesium disorder. Unlike Ba4Mo12S18 where some Mo6S8(i)S6(a) units are also connected through S(i-i) ligands, this connection mode does not lead to significant interactions in the title compound. Single-crystal resistivity measurements show that Cs(~1)Mo12S14 presents a metallic behavior with a superconducting transition at 7.7 K as confirmed by magnetic measurements.