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首页> 外文期刊>Zeitschrift fur Anorganische und Allgemeine Chemie >REACTIONS OF MONCL3 AND WNCL(3) WITH ELEMENTAL FLUORINE - CRYSTAL STRUCTURES OF MOO2F2(THF)(2) AND WF4(NCL)(CH3CN) German
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REACTIONS OF MONCL3 AND WNCL(3) WITH ELEMENTAL FLUORINE - CRYSTAL STRUCTURES OF MOO2F2(THF)(2) AND WF4(NCL)(CH3CN) German

机译：MONCL3 和 WNCL（3） 与元素氟的反应 - MOO2F2（THF）（2） 和 WF4（NCL）（CH3CN） 的晶体结构 德语

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The nitrido chlorides MoNCl3 and WNCl3 as well as WCl4(NCl) react with elemental fluorine forming the N-chloro imido complexes MoF4(NCl) and WF4(NCl), which were characterized by IR spectroscopy. With tetrahydrofurane MoF4(NCl) reacts to give MoF4(NCl)(THF), which in THF solution slowly converts into MoO2F2(THF)(2). From WF4(NCl) with acetonitrile the complex WF4(NCl)(CH3CN) is obtained. Both donor acceptor complexes were characterized by crystal structure determinations. MoO2F2(THF)(2): Space group P2(1)/n, Z = 4, structure solution with 1823 unique reflections, R = 0.033 for reflections with I > 2 sigma(I). Lattice dimensions at -40 degrees C: a = 636.2, b = 1119.5, c = 1625.2 pm; beta = 93.92(1)degrees. The compound has a monomeric molecular structure with the fluorine atoms in trans-position to one another and with the oxygen atoms of the THF molecules in trans to the oxo ligands. WF4(NCI)(CH3CN): Space group P2(1)/m, Z = 2, structure solution with 1119 unique reflections, R = 0.038 for reflections with I > 2 sigma(I). Lattice dimensions at 20 degrees C: a = 511.7, b = 714.9, c = 1002.5 pm; alpha = 102.59(10)degrees. The compound has a monomeric molecular structure in which the nitrogen atom of the acetonitrile molecule coordinates in trans-position to the N-chloro imido group W=N-Cl. The structural parameters of this group are WN = 172.2 pm, NCl = 161.1 pm, WNCl = 178.6 degrees. References: 28
机译：氮化氯MoNCl3和WNCl3以及WCl4（NCl）与元素氟反应生成N-氯酰亚胺配合物MoF4（NCl）和WF4（NCl），并用红外光谱表征了这些配合物。与四氢呋喃MoF4（NCl）反应生成[MoF4（NCl）（THF）]，在THF溶液中缓慢转化为[MoO2F2（THF）（2）]。由WF4（NCl）与乙腈制得络合物[WF4（NCl）（CH3CN）]。两种供体受体复合物均通过晶体结构测定进行表征。[MoO2F2（THF）（2）]：空间群P2（1）/n，Z = 4，具有1823个唯一反射的结构解，R = 0.033，用于I>2 sigma（I）的反射。-40°C时的晶格尺寸：a = 636.2，b = 1119.5，c = 1625.2 pm;贝塔 = 93.92（1）度。该化合物具有单体分子结构，氟原子相互转位，THF分子的氧原子反式到氧代配体。[WF4（NCI）（CH3CN）]：空间群 P2（1）/m，Z = 2，具有 1119 个唯一反射的结构解，R = 0.038 表示 I > 2 sigma（I） 的反射。20°C时的晶格尺寸：a = 511.7，b = 714.9，c = 1002.5 pm;阿尔法 = 102.59（10）度。该化合物具有单体分子结构，其中乙腈分子的氮原子以转位配位到N-氯酰亚胺基团W=N-Cl。该组的结构参数为 WN = 172.2 pm，NCl = 161.1 pm，WNCl = 178.6 度。[参考资料： 28]

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