N-Methylimidazolkomplexe des Berylliums: [Be(Me-Im)4]I2 und [Be3(μ-OH)3(Me-Im)6]Cl3
Résumé
Abstract. Tetra(N-methylimidazole)-beryllium-di-iodide, [Be(Me-Im)4]I2 (1), was prepared from beryllium powder and iodine in N-methylimidazole suspension to give yellow single crystal plates, which were characterized by X-ray diffraction and IR spectra. 1 crystallizes tetragonally in the space group I4¯2d with four formula units per unit cell. Lattice dimensions at 100(2) K: a = b = 1784.9(1), c = 696.2(1) pm, R1 = 0.0238. The structure consists of homoleptic dications [Be(Me-Im)4]2+ with short Be-N distances of 170.3(3) pm and iodide ions with weak interionic C-H...I contacts. Experiments to yield crystalline products from reactions of N-methylimidazole with BeCl2 and (Ph4P)2[Be2Cl6], respectively, in dichloromethane solutions were unsuccessful. However, single crystals of [Be3(μ-OH)3(Me-Im)6]Cl3 (2) were obtained from these solutions in the presence of moisture air. According to X-ray diffraction studies, two different crystal individuals (2a and 2b) result, depending on the starting materials BeCl2 and (Ph4P)2[Be2Cl6], respectively [2a: Space group P21/n, Z = 4; 2b: Space group P1¯, Z = 2]. As a side-product from the reaction of N-methylimidazole with (Ph4P)2[Be2Cl6] single crystals of (Ph4P)Cl*CH2Cl2 (3) were identified crystallographically (P21/n, Z = 4) which are isotypical with the corresponding known bromide (Ph4P)Br*CH2Cl2.
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