*Method 2: Microwave Irradiation*

To a solution of CuCl2·2H2O (0.9 mmol) in CH3CN (10 mL) was slowly added a solution of ligand (0.9 mmol) in CH3CN (10 mL). This mixture was irradiated for 10 min in a modified conventional microwave oven [31]. After slow evaporation at room temperature, we first isolated a few prismatic blue single crystals of **1**·**solv** and then blue plate single crystals of **1**. Yield: 69%.

### *Method 3: Stirring at Room Temperature*

To a solution of CuCl2·2H2O (0.9 mmol) in CH3CN (10 mL) was slowly added a solution of ligand (0.9 mmol) in CH3CN (10 mL). The mixture was stirred for 24 h at room temperature. The blue crystalline powder of **1** was filtered off and dried over CaCl2. Yield: 87%.

Data for **1**: MP: 170–175 ◦C. Anal. Calc. for C10H20Cl6N16O2S4Cu3: N 24.1%, C 13.0%, H 2.2%; Found: N 24.1%, C 13.2%, H 2.4%. IR (cm–1): 1480m, 1414m, 1393m, 1365m, ν(ring); 1177m, δ(CH); 1087m, 1039m, 1003m, δ(ring); 708s, ν(C–S).

### 4.2.2. [Cu2Cl2(BMTTE)]2 (2) and ∞2Cu2Cl4(BMTTE) (**3**)
