Facile Synthesis and Structures of Cyclic Triimidazole and Its Boric Acid Adduct

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• 作者：David M. Schubert ; Daniel T. Natan ; Duane C. Wilson ; Kenneth I. Hardcastle
• 刊名：Crystal Growth & Design
• 出版年：2011
• 出版时间：March 2, 2011
• 年：2011
• 卷：11
• 期：3
• 页码：843-850
• 全文大小：939K
• 年卷期：v.11,no.3(March 2, 2011)
• ISSN：1528-7505

文摘

Cyclic triimidazole, C₉H₆N₆ (1), was prepared by thermolysis of the easily prepared copper imidazolate framework solid, Cu(C₃H₃N₂)₂ (2), providing a convenient route to this potentially useful tecton for molecular design. Anhydrous 1 and a hydrate, 1路0.5H₂O, were characterized by single-crystal X-ray diffraction. Hydrate 1路0.5H₂O contains two crystallographically independent 1 molecules. Supramolecular structures of 1 and 1路0.5H₂O feature stacking arrangements in which the 1 molecule deviates from idealized geometry. A 3-fold H-bond acceptor 1 forms an adduct with boric acid, 1路B(OH)₃, which was also structurally characterized. This adduct is composed of hydrogen-bonded sheets of 1 and B(OH)₃ molecules with sheet interplanar separations of 3.175(4) 脜 and B(OH)₃ boron atoms positioned above and below the centroids of 1 in adjacent sheets. Unlike 1 and its hydrate, 1路B(OH)₃ contains 1 molecules that display crystallographically required D_3h symmetry. Anhydrous 1 crystallizes in the triclinic system, space group P1̅, with a = 7.2138(12), b = 8.3667(15), c = 8.8361(13) 脜, 伪 = 99.826(13), 尾 = 113.825(10), 纬 = 110.721(11)掳, V = 424.55(12) 脜³, Z = 2; 1₂路H₂O (or 1路0.5H₂O), triclinic, P1̅, a = 7.5608(3), b = 7.5669(5), c = 15.8436(8) 脜, 伪 = 84.504(3), 尾 = 81.269(3), 纬 = 87.038(3)掳, V = 891.18(8) 脜³, Z = 2; 1路B(OH)₃, trigonal, P3̅, a = 10.1186(3), b = 10.1186(3), c = 6.3488(4) 脜, 伪 = 90, 尾 = 90, 纬 = 120掳, V = 562.94(4) 脜³, Z = 2.