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70349966045
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note
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1.73 (X = OH, F). Calcd (wt%): C, 11.27; H, 3.15; N, 4.38; TG, 24.10. Found (wt%): C, 12.17; H, 3.20; N, 4.66; TG, 23.98.
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note
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2O (1.0 mL) and 2-methylpentamethylenediamine (MPMD, Dytel A, Sigma-Aldrich, 5.0 mL) with constant stirring. Then, 1,2-diaminopropane (1,2-PDA, 1.0 mL) and HF (40 wt %, 0.12 mL) were added to this mixture. A homogeneous gel was formed after stirring for ∼2 h. The gel was finally transferred to a 15-mL Teflon-lined stainless-steel autoclave and heated at 170°C for 12 days under static conditions. Colorless needle-shaped single crystals of JLG-12 were separated by filtration, washed with distilled water, and then dried in air. JLG-12 can also be obtained in the absence of 1,2-PDA. The addition of 1,2-PDA favored the formation of larger single crystals.
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70349954858
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note
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1 = 0.0938 for reflections with I > 2σ(I) and 0.1436 for all reflections.
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Blatov, V. A.; Delgado-Friedrichs, O.; O'Keeffe, M.; Proserpio, D. M. Acta Crystallogr., Sect. A 2007, 63, 418-425.
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O'Keeffe, M.3
Proserpio, D.M.4
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homepage at
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RCSR homepage at http://rcsr.anu.edu.au/.
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