Abstract

AbstractTetra(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 spectroscopy. Compound 1 crystallizes tetragonally in the space group I$\bar{4}$2d with four formula units per unit cell. Lattice dimensions at 100(2) K: a = b = 1784.9(1), c = 696.2(1) pm, R1 = 0.0238. The structure consists of homoleptic dications [Be(Me‐Im)4]2+ with short Be–N distances of 170.3(3) pm and iodide ions with weak interionic C–H···I contacts. Experiments to yield crystalline products from reactions of N‐methylimidazole with BeCl2 and (Ph4P)2[Be2Cl6], respectively, in dichloromethane solutions were unsuccessful. However, single crystals of [Be3(μ‐OH)3(Me‐Im)6]Cl3 (2) were obtained from these solutions in the presence of moisture air. According to X‐ray diffraction studies, two different crystal individuals (2a and 2b) result, depending on the starting materials BeCl2 and (Ph4P)2[Be2Cl6], respectively [2a: Space group P21/n, Z = 4; 2b: Space group P$\bar{1}$, 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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