Organic tin-inorganic tin hybrid Sn18 type crystalline tin-oxygen cluster compound and preparation method thereof
A technology of organotin and clusters, which is applied in the field of organotin-inorganic tin hybrid Sn18 crystalline tin-oxygen clusters and its preparation, which can solve the problems of structural diversity and insufficient functionality
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Embodiment 1
[0042] 5mmol benzoic acid, 0.5mmol phenylphosphonic acid, 0.1mmol SnCl 4 ·5H 2 O, 1 mmol of butyl stannoic acid and 7.5 mL of acetonitrile, water, and isopropanol mixed solution were loaded into a hydrothermal reaction kettle, and reacted at 100° C. for 3 days. The resulting mixed solution was filtered to obtain colorless blocky crystals. Washed with acetonitrile, filtered, and dried at room temperature, the organic tin-inorganic tin hybrid Sn 18 type crystalline tin-oxygen clusters with a yield of 78% (as SnCl 4 ·5H 2 O meter).
[0043] The analysis of the single crystal diffraction data of the colorless bulk crystal prepared in this example shows that the molecular formula of the complex is [(BuSn) 12 sn 6 (μ 3 -O) 20 (PhCO 2 ) 12 (PhPO 3 ) 4 ], the molecular weight is 5219.35, and the crystallographic data is α=90°, β=94.0540(10)°, γ=90°, Z=4, monoclinic system, P2 1 / c space group. Crystal structure such as figure 1 shown. In the crystal structure 18 Sn...
Embodiment 2
[0048] 5mmol p-toluic acid, 0.5mmol phenylphosphonic acid, 0.1mmol SnCl 4 ·5H 2 0, 1mmol of butyl stannoic acid and 7.5mL of acetonitrile, water, and isopropanol mixed solution were loaded into a hydrothermal reactor, and reacted for 4 days at 100°C. The resulting mixed solution was filtered to obtain colorless blocky crystals. Washed with acetonitrile, filtered, and dried at room temperature, the organic tin-inorganic tin hybrid Sn 18 type crystalline tin-oxygen cluster compound with a yield of 76% (as SnCl 4 ·5H 2 O meter).
[0049] The analysis of the single crystal diffraction data of the colorless bulk crystal prepared in this example shows that the molecular formula of the complex is [(BuSn) 12 sn 6 (μ 3 -O) 20 (4-MePhCO 2 ) 12 (PhPO 3 ) 4 ]·2CH 3 CN·2H 2 O, the molecular weight is 5500.21, the crystallographic data is α=76.2874(13)°, β=88.5702(11)°, γ=62.2587(15)°, Z=2, triclinic crystal system, space group P-1. Crystal structure such as Figure 5 ...
Embodiment 3
[0054] 5mmol p-tert-butylbenzoic acid, 0.5mmol phenylphosphonic acid, 0.1mmol SnCl 4 ·5H 2 O. 1mmol of butyl stannoic acid and 7.5mL of acetonitrile, water, and isopropanol mixed solution were charged into a hydrothermal reactor, and reacted at 100°C for 3 days. The resulting mixed solution was filtered to obtain colorless blocky crystals. Washed with acetonitrile, filtered, and dried at room temperature, the organic tin-inorganic tin hybrid Sn 18 type crystalline tin-oxygen cluster compound with a yield of 73% (as SnCl 4 ·5H 2 O meter).
[0055] In this example, the analysis of the diffraction data of the prepared colorless block crystal single crystal shows that the molecular formula of the complex is [(BuSn) 12 sn 6 (μ 3 -O) 20 (4-t-BuPhCO 2 ) 12 (PhPO 3 ) 4 ]·2CH 3 CN 2iPrO H 2H 2 O, the molecular weight is 6067.41, the crystallographic data is α=82.1576(12)°, β=80.6499(11)°, γ=67.7108(11)°, Z=2, triclinic crystal system, P-1 space group. Crystal str...
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