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The mixed tellurium/selenium Re6 clusters [NMe4]4[Re6(Te8 - n Se n )(CN)6] (n = 0−8) have been prepared from the reactions of Re6Te15 with the appropriate stoichiometry of NaCN and Se at 600 °C, followed by cation exchange with NMe4Br. A typical anion comprises an Re6 octahedron with its eight faces capped by μ3-chalcogen atoms to form a pseudocube, and each Re atom has a terminal cyanide ligand. These anions have essentially idealized cubic symmetry. In the [Re6Te8(CN)6]4- anion, Re−Re bond distances range from 2.673(1) to 2.690(1) Å and Re−(μ3-Te) distances range from 2.683(1) to 2.705(1) Å. In the [Re6Se8(CN)6]4- anion the Re−Re and Re−(μ3-Se) distances range from 2.622(2) to 2.638(2) Å and 2.520(3) to 2.550(3) Å, respectively. The “[Re6Te4.34Se3.66(CN)6]4-” anion, with disordered Se/Te positions, displays intermediate bond distances with Re−Re distances ranging from 2.653(1) to 2.665(1) Å and Re−(μ3-Q) (Q = Se, Te) distances ranging from 2.581(1) to 2.673(1) Å. Whereas single-crystal X-ray diffraction results provide the barest indication of the complicated nature of the mixed Te/Se crystalline products, NMR spectroscopy indicates that they comprise cations and mixtures of geometric isomers of [Re6(Te8 - n Se n )(CN)6]4- anions (125Te NMR (δ, ppm):  [NMe4]4[Re6Te8(CN)6], −1112; [NMe4]4[Re6Te7Se(CN)6], ≥10 peaks, −643 to −1231; [NMe4]4[Re6Te4Se4(CN)6], ≥18 peaks, −705 to −1234; [NMe4]4[Re6TeSe7(CN)6], ≥12 peaks, −648 to −1114. 77Se NMR (δ, ppm):  [NMe4]4[Re6TeSe7(CN)6], ≥8 peaks, 928 to 966; [NMe4]4[Re6Se8(CN)6]·31/3H2O, 933).

Three new compounds (enH)(6+n)Cu(40)Sn(15)S(60) (1), (enH)(3)Cu(7)Sn(4)S(12) (2), and (trenH(3))Cu(7)Sn(4)S(12) (tren = tris(2-aminoethyl)amine) (3) containing Cu(8)S(12) and Cu(7)SnS(12) clusters have been prepared from direct solvothermal reaction of the elements in amine solvents. In 1, the cubic close-packed arrangement of Cu(8)S(12) clusters, interconnected by capping SnS(4) tetrahedra and CuS(3) triangles, form two interpenetrating channel networks that are presumably filled with disordered solvent molecules. Structures 2 and 3 contain well-ordered, protonated amine molecules and Cu(7)SnS(12) clusters. The clusters are connected by SnS(4) tetrahedra to form a three-dimensional structure with ReO(3) topology. (119)Sn Mössbauer measurement is consistent with Sn(IV) atoms linking, and Sn(II) atoms within, the mixed-metal Cu(7)SnS(12) clusters.