1. Solventothermal Synthesis of Solid-State Chalcogenidometalates
2. Chalcogenidometalates of the heavier Group 14 and 15 elements
3. The compound Re4Te4(TeCl2)4Cl8was synthesized by a literature method.14A reaction mixture of Re4Te4(TeCl2)4Cl8(0.0233 g, 0.010 mmol), KSeCN (0.020 g, 0.14 mmol), and NH4Cl (0.10 g, 1.9 mmol) was loaded into a fused-silica tube under an Ar atmosphere in a glovebox. Then, 0.4 mL of acetonitrile was added via syringe. The tube was frozen, evacuated to ∼10-3Torr, flame-sealed, and thawed. It was then loaded into a high-pressure autoclave along with 1700 mL of H2O to counter the pressure. The autoclave was heated at 200 °C for 3 days and then cooled to room temperature. Orange crystals of [(CH3)C(NH2)2]4[Re6Se8(CN)6] were recovered by suction filtration and washed with acetone. Yield of crystals was 0.007 g (50% based on Re). A second preparation afforded a yield of 40% based on Re. Examination of these crystals with an EDX-equipped Hitachi S-3500 SEM gave Re/Se = 3:4. The compound is stable in air.
4. Cocrystallized Mixtures and Multiple Geometries: Syntheses, Structures, and NMR Spectroscopy of the Re6 Clusters [NMe4]4[Re6(Te8-nSen)(CN)6] (n = 0−8)