Research Article
Synthesis, Structure, and Cyclocondensation of the 4,4,4-Trifluoro-3,3-dihydroxy-2-methyl-1-(thien-2-yl)-1-butanone with Hydroxylamine and Hydrazine
Table 1
Crystallographic data and structure refinement parameters of 3.
| | Chemical formula | C9 H9 F3 O3 S |
| | Mass weight | 254.22 | | Temperature | 293 K | | Wavelength | 0.71073 Å | | Crystal system | Monoclinic | | Space group | P 21/n | | Unit cell dimensions | Å,
Å, °
Å, | | Volume | 1080.67(11) Å3 | | Z | 4 | | Density (calculated) | 1.563 mg/m3 | | F(000) | 520 | | Crystal size | 0.45 × 0.33 × 0.27 mm3 | | Theta range for data collection | 3.24 to 28.20° | | Index ranges | −8 ≤ h ≤ 8, −10 ≤ k ≤ 10, −28 ≤ l ≤ 28 | | Reflections collected | 25372 | | Independent reflections | 2636 [R(int) = 0.0597] | | Completeness to theta = 27.27° | 98.9% | | Refinement method | Full-matrix least-squares on F2 | | Computing | COLLECT, HKL Denzo and Scalepack, SHELXS-97, SHELXL-97 | | Data/restraints/parameters | 2636/0/145 | | Goodness-of-fit on F2 | 1.059 | | Final R indices [I > 2σ(I)] | R1 = 0.0457, wR2 = 0.1114 | | R indices (all data) | R1 = 0.0634, wR2 = 0.1216 | | Largest diff. peak and hole | 0.255 and −0.326 e.Å−3 |
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