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Metal acetates and organostibonic acids (1:1 ratio) were dissolved in acetonitrile (10 mL) and reacted in presence of base (pyridine or triethylamine) in ambient conditions (for 2) or under solvothermal conditions at 100 °C (for 1, 3, 4, and 5). For 1-3, this gave the products in moderate yields. Crystals were obtained either by slow evaporation of the solvent at room temperature or directly by slow cooling of the Teflon container used for solvothermal synthesis.
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Metal acetates and organostibonic acids (1:1 ratio) were dissolved in acetonitrile (10 mL) and reacted in presence of base (pyridine or triethylamine) in ambient conditions (for 2) or under solvothermal conditions at 100 °C (for 1, 3, 4, and 5). For 1-3, this gave the products in moderate yields. Crystals were obtained either by slow evaporation of the solvent at room temperature or directly by slow cooling of the Teflon container used for solvothermal synthesis.
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It is important to stress that the structures reported here contain disordered ligands and solvent-accessible voids in which solvent can be severely disordered. Details of the structural problems are given in the Supporting Information. Structural details for 1: orthorhombic, Pcca, a, 38.11. b, 25.37, c, 27.18 Å, R, 0.0649. For 2: monoclinic, P21/c, a, 19.39, b, 25.82, c, 22.62 Å, β, 101.24°, R, 0.0722. For 4: monoclinic, C2/c, a, 31.87. b, 17.85, c, 28.47 Å, β, 118.11°, R, 0.0671. For 5: triclinic, P1, a, 19.22, b, 21.16, c, 29.44 Å, α, 104.84°, β, 100.52°, γ, 96.96°, R, 0.0677. Microanalysis for 1. Calcd: C, 26.00; H, 2.54: N, 0.0. Found: C, 26.45; H, 2.72; N, 0.0. For 2. Calcd: C, 29.53; H, 2.50; N, 1.23. Foun
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1/c, a = 19.39, b = 25.82, c = 22.62 Å, β = 101.24°, R = 0.0722. For 4: monoclinic, C2/c, a = 31.87. b = 17.85, c = 28.47 Å, β = 118.11°, R = 0.0671. For 5: triclinic, P1, a = 19.22, b = 21.16, c = 29.44 Å, α = 104.84°, β = 100.52°, γ = 96.96°, R = 0.0677. Microanalysis for 1. Calcd: C, 26.00; H, 2.54: N, 0.0. Found: C, 26.45; H, 2.72; N, 0.0. For 2. Calcd: C, 29.53; H, 2.50; N, 1.23. Found: C, 26.85; H, 2.65; N, 1.45.
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