Source of materialThe title compound was synthesized under solvothermal condition, in which pyridine was both the solvent and a reactant. A mixture of boric acid (4.091 g), diethylenetriamine (2.0 ml), tetraethylenepentamine (2.0 ml), pyridine (5.0 ml) and distilled water (0.1 ml) sealed in a 15 ml Teflon-lined stainless-steel vessel and heated at 170°C for 7 days, and then cooled to room temperature. The resulting solid powder was collected by filtration and washed thoroughly with absolute alcohol. The mixture of the obtained solid powder (0.755 g), H 3BO3 (0.786 g), pyridine (5.0 ml) and distilled water (0.1 ml) was sealed in a 15 ml Teflon-lined stainless-steel vessel again and heated at 150°C for 5 days and then cooled to room temperature. The resulting colorless transparent crystals were recovered. They were sealed in a capillary together with mother solution because of their instability in the air. Experimental detailsThe low Ngt/Nparam ratio is caused by the poor quality of the crystals which is probably connected with the disorder of the solvent. anions both electrostatically and via NH···O hydrogen bonds. Discussion
C 16H16BNO6, orthorhombic, Aba2 (no. 41), a = 8.544(7) Å, b = 19.68(2) Å, c = 9.117(7) Å, V = 1532.9 Å 3 , Z = 4, R gt(F) = 0.052, wRref(F 2 ) = 0.136, T = 298 K. Source of materialThe title compound was synthesized using DMF as the solvent. Boric acid (0.13 g, 2.16 mmol) was added to a stirred solution of salicylic acid (0.64 g, 4.65 mmol) in dry DMF (10.0 ml). The reaction mixture was stirred at 125°C for 48 h. The DMF solvent was removed by evaporation under reduced pressure, then acetone (5.0 ml) was added, the brown and viscous substance was dissolved and the solution became clear. Finally, ether (5.0 ml) was added, the resulting colorless powder was crystallized and filtered after 3 h at room temperature. can also be expressed as BL2 form (H 2L = salicylic acid). The sp 3 -hybridized B atom is bonded to four oxygen atoms to form a tetrahedral environment. The BO distances range from 1.428 (5) are discrete units. They interact both electrostatically and via NH···O hydrogen bonds with N···O distances in the range 3.177 Å 3.194 Å ( figure, bottom). The dimethylformamide acts not only as the solvent, but also as a reactant. It decomposes under experimental conditions and forms the [(CH 3)2NH2] + cations.
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