[HCB _(11)Cl _(11)] - Synthesis, characterization, crystal structure, and reaction with P _4

Bolli C.; K?chner T.; Knapp C.

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[HCB _(11)Cl _(11)] - Synthesis, characterization, crystal structure, and reaction with P _4

机译：[HCB _（11）Cl _（11）]-合成，表征，晶体结构和与P _4的反应

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The thermodynamic stability of the [HCB _(11)Cl _(11)] ~- salts of the cationic one-electron oxidizers [NO] ~+ and [O _2] ~+ was estimated by Born-Haber-Fajans cycles based on quantum-chemical calculations and lattice enthalpy estimations. [NO][HCB _(11)Cl _(11)] is predicted to be a stable compound, whereas [O _2][HCB _(11)Cl _(11)] should decompose into O _2 and the HCB _(11)Cl _(11) · radical. Consequently, [NO][HCB _(11)Cl _(11)] can be prepared by metathesis reaction from Na[HCB _(11)Cl _(11)] and [NO][BF _4] in liquid sulfur dioxide, while attempts to synthesize [O _2][HCB _(11)Cl _(11)] failed. [NO][HCB _(11)Cl _(11)] has been fully characterized by NMR and vibrational spectroscopy. Single crystals of [NO][HCB _(11)Cl _(11)]·SO _2 were obtained from liquid sulfur dioxide solution. The crystal structure determination revealed several intermolecular cation-anion contacts, which are significantly shorter than the sum of the van der Waals radii of the respective atoms. [NO][HCB _(11)Cl _(11)] reacts with white phosphorus in CH _2Cl _2 solution to give yellow-orange [P _4NO][HCB _(11)Cl _(11)] containing the [P _4NO] ~+ cation. An in-situ NMR spectroscopic study indicates the presence of the homopolyatomic phosphorus cation [P _9] ~+ in the reaction mixture.

机译：阳离子单电子氧化剂[NO]〜+和[O _2]〜+的[HCB _（11）Cl _（11）]〜-盐的热力学稳定性通过Born-Haber-Fajans循环基于量子化学计算和晶格焓估计。预测[NO] [HCB _（11）Cl _（11）]是稳定的化合物，而[O _2] [HCB _（11）Cl _（11）]应该分解为O _2和HCB _（ 11）Cl _（11）·自由基。因此，在液态二氧化硫中，由Na [HCB _（11）Cl _（11）]和[NO] [BF _4]通过复分解反应可以制备[NO] [HCB _（11）Cl _（11）]，尝试合成[O _2] [HCB _（11）Cl _（11）]失败。 [NO] [HCB _（11）Cl _（11）]已通过NMR和振动光谱法充分表征。从液态二氧化硫溶液获得[NO] [HCB _（11）Cl _（11）]·SO _2的单晶。晶体结构的确定揭示了几个分子间阳离子-阴离子接触，它们明显短于各个原子的范德华半径之和。 [NO] [HCB _（11）Cl _（11）]与白色磷在CH _2Cl _2溶液中反应，生成橙黄色的[P _4NO] [HCB _（11）Cl _（11）]，其中含有[P _4NO ]〜+阳离子。原位NMR光谱研究表明，反应混合物中存在同多原子磷阳离子[P _9]〜+。

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《Zeitschrift fur Anorganische und Allgemeine Chemie》 |2012年第4期|共6页
作者
Bolli C.; K?chner T.; Knapp C.;
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正文语种 eng
中图分类化学;
关键词
Carborates; Nitrosyl cation; Phosphorus; Polyatomic main group cations; Weakly coordinating anions;

机译：硼酸根;亚硝酰基阳离子;磷;多原子主族阳离子;弱配位阴离子;

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[HCB _(11)Cl _(11)] - Synthesis, characterization, crystal structure, and reaction with P _4

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