Wuttke Stefan, Lehmann Anja, Scholz Gudrun, Feist Michael, Dimitrov Anton, Troyanov Sergey I, Kemnitz Erhard
Institut für Chemie, Humboldt-Universität zu Berlin, Brook Taylor Str. 2, D-12489, Berlin, Germany.
Dalton Trans. 2009 Jun 28(24):4729-34. doi: 10.1039/b901030k. Epub 2009 Apr 29.
The structures of magnesium methoxide and magnesium methoxide fluoride obtained via the reaction of Mg(OCH(3))(2) with HF were investigated by single-crystal structure analysis and multinuclear solid-state NMR ((13)C and (19)F). The fluorolysis of magnesium methoxide transforms the cubane structure units in hexanuclear dicubane units containing micro(4)-fluorine atoms. The resulting Mg(6)F(2)(OCH(3))(10)(CH(3)OH)(14) compound crystallizes in two different crystalline modifications. Moreover by slow thermal decomposition of the compound Mg(6)F(2)(OCH(3))(10)(CH(3)OH)(14), it loses two outer CH(3)OH molecules and leaves crystal structure Mg(6)F(2)(OCH(3))(10)(CH(3)OH)(12). The thermal behavior of Mg(OCH(3))(2)(CH(3)OH)(3.55) and Mg(6)F(2)(OCH(3))(10)(CH(3)OH)(14) was investigated by DTA and XRD. Both compounds lose the solvated methanol completely by heating above 150 degrees C and form MgO above 600 degrees C as well as amorphous MgF(2) in the case of magnesium methoxide fluoride.
通过单晶结构分析和多核固态核磁共振（¹³C和¹⁹F）研究了由Mg(OCH(3))(2)与HF反应得到的甲醇镁和甲醇镁氟化物的结构。甲醇镁的氟解作用将六核双立方烷单元中的立方烷结构单元转化为含有μ(4)-氟原子的单元。所得的Mg(6)F(2)(OCH(3))(10)(CH(3)OH)(14)化合物以两种不同的晶体变体结晶。此外，通过对化合物Mg(6)F(2)(OCH(3))(10)(CH(3)OH)(14)进行缓慢热分解，它失去两个外部的CH(3)OH分子，留下晶体结构Mg(6)F(2)(OCH(3))(10)(CH(3)OH)(12)。通过差示热分析（DTA）和X射线衍射（XRD）研究了Mg(OCH(3))(2)(CH(3)OH)(3.55)和Mg(6)F(2)(OCH(3))(10)(CH(3)OH)(14)的热行为。两种化合物在加热到150℃以上时都会完全失去溶剂化甲醇，在甲醇镁氟化物的情况下，在600℃以上会形成MgO以及无定形MgF(2)。
