Na2[(mu-N,N'-C10H12N2O8)(mu-O)(mu-S)-Mo2O2].2H2O.

Na2[(mu-N,N'-C10H12N2O8)(mu-O)(mu-S)-Mo2O2].2H2O.
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Na2[(mu-N,N-C10H12N2O8)(mu-O)(mu-S)-Mo2O2].2H2O。

DOI:
10.1107/s0108270198003163
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发表时间:
1998
期刊:
Acta crystallographica. Section C, Crystal structure communications
影响因子:
--
通讯作者:
Hicks,KW
Hicks,KW
中科院分区:
--
文献类型:
--
作者:
Valente,EJ;Zubkowski,JD;Hicks,KW

文献摘要

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硫化物取代一个或两个桥的二钼(V)桥氧配合物的类似物是已知的。在无氧条件下,[(MoO_3)_2(EDTA)]_4·μ-(ethylenediaminetetraacetato)-μ-oxo-μ-sulfido-bis[oxomolybdenum(V)](μ为乙二胺四乙酸酯)在pH=6的条件下与二亚硫酸盐还原后,用原位生成的硫化物缓慢置换桥氧化物,得到标题化合物−_2[Mo2O_3S(C_10H_12N_2O_8)]·2H2O。红外光谱分析和核磁共振光谱分析与不对称络合物一致。在分子结构中,Mo中心具有扭曲的八面体配位,平均Mo-S距离为2.320 (1) ?,平均桥联Mo-O距离为1.938 (3) ?Mo-⋯-Mo接触距离[2.666 (1) ä]介于可比的di-μ-oxo和di-μ-Sulfido络合物之间。Na+离子的配位球中分别有五个和六个最近的O原子,每个配位球中都有一个无序的水氧。
Analogs of bridging-oxo complexes of dimolybdenum(V) where sulfide replaces one or both bridges are known. After reduction of [(MoO3)2(μ-edta)]4− (edta is ethylenediaminetetraacetate) with dithionite at pH 6 in the absence of dioxygen, slow replacement of bridging oxide with sulfide produced in situ produces the title compound, disodium μ-(ethylenediaminetetraacetato)-μ-oxo-μ-sulfido-bis[oxomolybdenum(V)] dihydrate, Na2[Mo2O3S(C10H12N2O8)].2H2O]. IR and NMR spectroscopic analyses are consistent with an unsymmetrical complex. In the molecular structure, the Mo centers have distorted octahedral coordination, with an average Mo—S distance of 2.320 (1) Å and an average bridging Mo—O distance of 1.938 (3) Å. The Mo⋯Mo contact distance [2.666 (1) Å] is intermediate between those in comparable di-μ-oxo and di-μ-sulfido complexes. Na+ ions have five and six nearest O atoms, respectively, in their coordination spheres, which each include one disordered water oxygen.