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首页> 外文期刊>Zeitschrift fur Anorganische und Allgemeine Chemie >Syntheses, structures, and polymorphism of beta-diketonato complexes - Co(thd)(3)
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Syntheses, structures, and polymorphism of beta-diketonato complexes - Co(thd)(3)

机译：β-二酮体复合物的合成，结构和多态性-Co（thd）（3）

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Oxidation of Co(thd)(2) dissolved in different solvents has been investigated in air and oxygen atmosphere. In oxygen atmosphere and at the boiling point of the solvents this treatment leads to oxidation of Coll to Co-III, but also to degradation of some of the thd ligands and formation of a new mixed-ligand complex. Three pure-cultivated crystalline Co(thd)(3) phases are reported: 1 (room-temperature phase), 2 (low-temperature phase), and 3 (metastable phase) and in addition there exists an amorphous Co(thd)(3) phase (4) with approximate composition Co(thd)(3) center dot xH(thd); x = 0.06. Reaction of metal(II) oxides (MO, M = Mn, Fe, and Co) with H(thd) under air or O-2 atmosphere is an easy direct route to M(thd)(3) complexes. Structure determinations are reported for Co(thd)(3) (1-3) based on single-crystal X-ray diffraction data. Modification 1 crystallizes in space group P (3) over bar c1 with a = b = 18.8100(10), c = 8.815(2) angstrom at 295 K; R(wR2) = 0.180, modification 2 in space group C2/c with a = 28.007(12), b = 18.482(8), c = 21.356(9) angstrom, 0 = 97.999(5)degrees at 100 K; R(wR2) =0.211, and modification 3 in space group Pnma with a = 19.2394(15) b = 18.8795(15), c = 10.7808(8) A at 100 K; R(wR2) = 0.193. The molecular structures of 1-3 all comprise a central Co atom octahedrally co-ordinated by the ketonato O atoms of three thd ligands. The transformation between modifications 1 and 2 is of a fully reversible second-order character. Modifications 1 and 3 are, oil the other hand, related by a quasi-reversible cycle. Heat treatment (specifically sublimation) of 1 leads to 3 whereas re-crystallization or prolonged storage at room temperature is required to regenerate 1. Co(thd)(3) has sufficient thermal stability to permit sublimation without degradation. The various forms of Co(thd)(3) are all diamagnetic, viz. a confirmation of the Co-III valence state.
机译：已经研究了在空气和氧气气氛中溶解在不同溶剂中的Co（thd）（2）的氧化作用。在氧气气氛中和在溶剂的沸点下，该处理导​​致Coll氧化为Co-III，而且还导致某些thd配体降解并形成新的混合配体配合物。报告了三种纯培养的结晶Co（thd）（3）相：1（室温相），2（低温相）和3（易位相），此外还存在无定形Co（thd）（ 3）具有近似组成Co（thd）（3）中心点xH（thd）的相（4）; x ＝ 0.06。金属（II）氧化物（MO，M = Mn，Fe和Co）在空气或O-2气氛下与H（thd）的反应是直接生成M（thd）（3）配合物的简便方法。基于单晶X射线衍射数据报道了Co（thd）（3）（1-3）的结构确定。修改1在棒c1上的空间群P（3）中结晶，在295 K时a = b = 18.8100（10），c = 8.815（2）埃; R（wR2）= 0.180，空间群C2 / c中的修改2，a = 28.007（12），b = 18.482（8），c = 21.356（9）埃，0 = 97.999（5）度，在100 K; R（wR2）= 0.211，空间群Pnma中的修改3，在100 K时a = 19.2394（15）b = 18.8795（15），c = 10.7808（8）A; R（wR2）= 0.193。 1-3的分子结构都包含一个中心Co原子，该中心Co原子由三个thd配体的酮基O原子八面体配位。修改1和2之间的转换具有完全可逆的二阶特征。另一方面，修改例1和3与准可逆循环有关。热处理（特别是升华）为1会导致3，而再生（1）需要在室温下进行重结晶或长时间存放才能再生。Co（thd）（3）具有足够的热稳定性，可以升华而不降解。 Co（thd）（3）的各种形式都是抗磁性的，即。确认Co-III价态。

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