Reiss Guido J, Boldog Ishtvan, Janiak Christoph
Institut für Anorganische Chemie und Strukturchemie, Heinrich Heine Universität Düsseldorf, Universitätsstrasse 1, D-40225 Düsseldorf, Germany.
Acta Crystallogr Sect E Struct Rep Online. 2011 Aug 1;67(Pt 8):m1109-10. doi: 10.1107/S1600536811027073. Epub 2011 Jul 23.
The crystal structure of the title compound, [Mg(C(3)H(7)NO)(4)(H(2)O)(2)]Cl(2), in which the Mg ion lies on a crystallographic inversion centre, confirms that of the previous room-temperature study [Pavanello et al. (1995 ▶). Main Group Met. Chem.18, 9-19]. This redetermination at 113 K has improved geometry precision by almost an order of magnitude [e.g. Mg-O(w) (w = water) distances = 2.094 (4) and 2.0899 (7) Å in the old and new structures, respectively] and allowed the water H atoms to be located and their positions refined. In the crystal, O-H⋯Cl hydrogen bonds between the two aqua ligands of the complex mol-ecule and neighboring chloride counter-anions generate supra-molecular chains propagating along [010]. The dicationic [Mg(DMF)(4)(H(2)O)(2)] unit (DMF is dimethyl-formamide) adopts a slightly distorted octa-hedral geometry in which the Mg atom is coordinated by four DMF O atoms in a pseudo-tetra-gonal arrangement and two trans aqua ligands.
标题化合物[Mg(C₃H₇NO)₄(H₂O)₂]Cl₂的晶体结构中,镁离子位于晶体学反演中心,这证实了之前室温研究[Pavanello等人,(1995 ▶)。主族金属化学,18,9 - 19]的结果。在113 K下的重新测定使几何精度提高了近一个数量级[例如,旧结构和新结构中Mg - O(w)(w = 水)的距离分别为2.094(4)和2.0899(7) Å],并使得水分子中的氢原子得以定位并精修其位置。在晶体中,配合物分子的两个水合配体与相邻的氯离子反离子之间的O - H⋯Cl氢键形成了沿[010]方向延伸的超分子链。二价阳离子[Mg(DMF)₄(H₂O)₂]单元(DMF为二甲基甲酰胺)采用略微扭曲的八面体几何构型,其中镁原子由四个呈假四方排列的DMF O原子和两个反式水合配体配位。