A new copper−antimony sulfide, [C4H12N2]0.5[CuSb6S10], has been hydrothermally synthesized from binary metal sulfides in the presence of triethylenetetramine and characterized by single-crystal X-ray diffraction, thermogravimetry, elemental analysis, and SQUID magnetometry. The product (Mr = 1158.72) crystallizes in the monoclinic space group P21/n with a = 11.2578(4) Å, b = 12.5259(5) Å, c = 13.9390(7) Å, β = 102.445(3)°, and V = 1919.4 Å3. The structure consists of cyclic Sb3S63- units in a boatlike conformation, linked by Sb−S bonds to form a complex Sb6S126- building block. Sb−S bonds serve to link Sb6S126- units to four others in a herringbone array, forming a sheet of stoichiometry Sb6S102-, containing 24-membered rings of alternating Sb and S atoms. Pairs of edge-sharing CuS4 distorted tetrahedra form pillars which link Sb6S102- layers together. The interlayer space contains piperazine cations, formed by cyclization of the triethylenetetramine during synthesis. Bond-valence sums are consistent with the presence of antimony(III) and copper(I), requiring complete protonation of the amine.
No takes yet. Share an insight, caveat, or question.
Powell et al. (2002) studied this question.