Abstract
Hydrothermal methods were developed for the growth of large, 3 mm-sized crystals of pyridine dodecasil-3C (Py-D3C) from a pyridine-SiO2-HF-H2O system at 190°C. The crystals were acentric at ambient temperature and were weak second harmonic generators. Phase transformations were observed by differential scanning calorimetry to commence at 161 and -46 °C on cooling. The crystal structure of the ambient temperature tetragonal or pseudotetragonal I7SiO2·C5H5N phase was determined using single crystal X-ray diffraction techniques [ a = 13.6620(5) Å, c = 19.5669(7) Å, . = 4, space group I42d- D122d]. The domain structure of this phase was studied using optical microscopy, and domain configurations were manipulated by heat treatment. Scanning electron micrographs strongly suggested that the boundaries of these domains were associated with growth twin boundaries.
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