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2O (10 mL) in a molar ratio of 1:12.3: 1.5:341 heated in a 23-mL acid digestion bomb at 170°C for 66 h gave 0.20 g black plates of 1.
-
-
-
-
22
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2842582552
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note
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3, and Z = 4. Data were collected on an AFC7R diffractometer with Mo Ka radiation (λ = 0.7106 Å) and a 18 kW rotating anode generator at room temperature. Structure solution and refinement by full-matrix least-squares using teXsan program package based on 1977 reflections with I ≥ 3σ(1) and 172 variables gave R(Rw) = 0.040 (0.043). All of the non-hydrogen atoms were refined anisotropically All of the hydrogen atoms were located from difference Fourier maps and included in the refinement with fixed positional and thermal parameters.
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27
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