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首页> 外文期刊>Zeitschrift fur Anorganische und Allgemeine Chemie >Syntheses and Crystal Structures of the Nitrido-chloro-molybdates [Mg(THF)_4{NMoCL_4(THF}_2] centre dot 4CH_2Cl_2 and [Li(12-Crown-4)(NMoCl_4)]_2 centre dot 2CH_2Cl_2
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Syntheses and Crystal Structures of the Nitrido-chloro-molybdates [Mg(THF)_4{NMoCL_4(THF}_2] centre dot 4CH_2Cl_2 and [Li(12-Crown-4)(NMoCl_4)]_2 centre dot 2CH_2Cl_2

机译：硝化氯钼酸盐[Mg（THF）_4 {NMoCL_4（THF} _2]中心点4CH_2Cl_2和[Li（12-Crown-4）（NMoCl_4）] _ 2中心点2CH_2Cl_2的合成和晶体结构

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摘要

Both the title compounds as well as [Li(12-crown-4)_2]~+MoNCl~- were made from MoNCl_3 and the chlorides MgCl_2 and LiCl, respectively, in dichloromethane suspensions in the presence of tetrahydrofuran and 12-crown-4, respectively. They form orange-red moisture-sensitive crystals, with were characterized by their IR spectra and partly by crystal structure analyses. [Mg(THF)_4{NMoCl_4(THF)}_2] centre dot 4CH_2Cl_2 (1): space group C2/m, Z = 2, lattice dimensions at -50 deg C: a = 1726.6(1), b = 1194.8(1), c = 1293.5(2) pm; #beta# = 90.87(1) deg; R1 = 0.037. In 1 the magnesium ion is coordinated octahedrally by the oxygen atoms of the four THF molecules and in trans-position by the nitrogen atoms of the two [N ident to MoCl_4(THF)]~- ions. [Li(12-crown-4)(NMoCl_4)]_2 centre dot 2CH_2Cl_2 (2): space group P1, Z = 1, lattice dimensions at -70 deg C: a = 930.4(1), b = 957.9(1), c = 1264.6(1) pm; #alpha# =68.91(1) deg, #beta# = 81.38(1), #gamma# = 63.84(1) deg; R1 = 0.0643. 2 forms a centrosymmetric ion ensemble in the dimeric cation of which, i.e. [Li(12-crown-4)]_2~(2+), the lithium ions on the one hand are connected to the four oxygen atoms each of the crown ether molecules in a was not yet known; and in addition, each of the lithium ions enters into a intermolecular Li-O bond with neighboring crown ether molecules under formation of a Li_2O_2 fourmembered ring. The two N ident to MoCl_4~- counterions are loosely coordinatd to one oxygen atom each of the crown ether molecules with Mo-O distances of 320.2 pm.
机译：标题化合物以及[Li（12-crown-4）_2]〜+ MoNCl〜-均由MoNCl_3以及氯化物MgCl_2和LiCl分别在四氢呋喃和12-crown-4的二氯甲烷悬浮液中制得。 ， 分别。它们形成橙红色的湿敏晶体，其特征在于其红外光谱，部分通过晶体结构分析来表征。 [Mg（THF）_4 {NMoCl_4（THF）} _ 2]中心点4CH_2Cl_2（1）：空间群C2 / m，Z = 2，在-50摄氏度下的晶格尺寸：a = 1726.6（1），b = 1194.8（ 1），c = 1293.5（2）pm; ＃beta＃= 90.87（1）度; R1 = 0.037。在1中，镁离子由四个THF分子的氧原子八面体配位，并且由两个[与MoCl_4（THF）]-离子相同的氮原子转位。 [Li（12-crown-4）（NMoCl_4）] _ 2中心点2CH_2Cl_2（2）：空间群P1，Z = 1，-70℃时的晶格尺寸：a = 930.4（1），b = 957.9（1） ，c = 1264.6（1）pm; ＃alpha＃= 68.91（1）度，＃beta＃= 81.38（1），＃gamma＃= 63.84（1）度; R1 = 0.0643。 2在其二聚阳离子即[Li（12-crown-4）] _ 2〜（2+）的二聚阳离子中形成一个中心对称离子集合体，锂离子一方面与每个冠醚的四个氧原子相连尚不知道a中的分子;另外，在形成Li_2O_2四元环的情况下，各锂离子与相邻的冠醚分子进入分子间的Li-O键。 MoCl_4--的两个N离子与一个氧原子松散配位，每个冠醚分子的Mo-O距离为320.2 pm。

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