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首页> 外文期刊>Chemistry: A European journal >The first examples of a crown ether intramolecularly encapsulating mono- and diorganotin dications: Synthesis and structures of [PhSnCH _2([16]crown-5)][ClO_4]_2and [HOSnCH _2([16]crown-5)][Y]_2 (Y = ClO_4, CF _3so_3)
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The first examples of a crown ether intramolecularly encapsulating mono- and diorganotin dications: Synthesis and structures of [PhSnCH _2([16]crown-5)][ClO_4]_2and [HOSnCH _2([16]crown-5)][Y]_2 (Y = ClO_4, CF _3so_3)

机译：冠醚分子内包封单和双有机锡药物的第一个实例：[PhSnCH _2（[16] crown-5）] [ClO_4] _2和[HOSnCH _2（[16] crown-5）] [Y]的合成和结构_2（Y = ClO_4，CF _3so_3）

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摘要

The reaction of silver Perchlorate with [PhI_2SnCH _2([16]crown5)] (1) and [I_3SnCH_2([16]crown-5)] (2) gave the organotin(IV)-substituted crown ether complexes [PhSnCH _2([16]crown-5)][ClO_4]_2 (3) and [HOSnCH _2([16]crown-5)][Y]_2 (4: Y = ClO_4, 5: Y = CF_3SO_3), respectively. All compounds have been isolated as airstable materials and characterised by ~1H, ~(13)C, ~(119)Sn and ~(119)Sn MAS (5) NMR spectroscopy, ESIMS spectrometry, elemental analysis and by single-crystal Xray diffraction analysis. The molecular structures of 3-5 show that the tin(IV) cation fits perfectly into the crown ether cavity and is coordinated by the five oxygen atoms of the ring to give a pentagonal bipyramidal configuration about the central metal cation. Notably, compounds 4 and 5 contain the first monomeric monoorganotin dication. Moreover, there are ~3J(~1H, ~(119)Sn) coupling constants to the CH_2CH proton of 377 (3) and 470 Hz (4, 5) that are, to the best of our knowledge, the biggest such couplings ever reported.
机译：高氯酸银与[PhI_2SnCH _2（[16] crown5）]（1）和[I_3SnCH_2（[16] crown-5）]（2）的反应得到有机锡（IV）取代的冠醚配合物[PhSnCH _2（[ 16] crown-5）] [ClO_4] _2（3）和[HOSnCH _2（[16] crown-5）] [Y] _2（4：Y = ClO_4，5：Y = CF_3SO_3）。所有化合物均已被分离为可挥发的材料，并通过〜1H，〜（13）C，〜（119）Sn和〜（119）Sn MAS进行表征（5）NMR光谱，ESIMS光谱，元素分析和单晶X射线衍射分析。 3-5的分子结构表明，锡（IV）阳离子完全适合冠醚腔，并与环中的五个氧原子配位，形成围绕中心金属阳离子的五角双锥体构型。值得注意的是，化合物4和5含有第一单体单有机锡指示剂。此外，与377（3）和470 Hz（4，5）的CH_2CH质子有〜3J（〜1H，〜（119）Sn）耦合常数，据我们所知，这是有史以来最大的此类耦合报告。

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