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首页> 外文期刊>Chemistry: A European journal >Nucleation-Controlled Crystallization of a New, Spontaneously Resolved Solvate of [Ru(bpy)_3](PF_6)_2 and its Desolvation Reaction
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Nucleation-Controlled Crystallization of a New, Spontaneously Resolved Solvate of [Ru(bpy)_3](PF_6)_2 and its Desolvation Reaction

机译：[Ru（bpy）_3]（PF_6）_2的新自发溶剂化的成核控制结晶及其去溶剂化反应

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摘要

Simply by increasing the supersaturation level, racemic [Ru(bpy)_3](PF_6)_2 no longer crystallises as the well-known true racemate (beta-modification; P3c1, a = 10.6453(5), c = 16.2987(9) A, Z = 2). Rather, it spontaneously resolves and forms a conglomerate resolves and forms a conglomerate of pure LAMBDA-and pure DELTA-crystals with a so far unknown structure type. This new modification actually is a solvate ([Ru(bpy)_3](PF_6)_2·1.5CH_3COCH_3; delta-type; P32, a = 13.8133(7) A, c = 11.6523(7) A, Z =2). By a solution-mediated equilibrium the new modification is shown to be the metastable (Ostwald) product, which is formed based on nucleation kinetics. Uon desolvation the solvate transforms into a second enantiomorphic crystal structure (gamma-type; P3_1, a = 10.3809(4), c = 26.2576(13)A, Z = 3). The latter could previously only be obtained by chemical resolution prior to crystallisation, but could not be accessed directly from racemic solutions. However, the new delta-modification can now be utilised for optical resolution by the so-called method of "resolution of entrainment". This example emphasises the potential that both kinetically controlled crystallisation and desolvation of solvates bear with respect to crystal engineering.
机译：只需增加过饱和水平，外消旋[Ru（bpy）_3]（PF_6）_2就不再像众所周知的真正外消旋体一样结晶（β-修饰; P3c1，a = 10.6453（5），c = 16.2987（9）A ，Z = 2）。而是，它自发地分解并形成了团块，并分解并形成了迄今结构类型未知的纯LAMBDA和纯DELTA晶体的团块。此新修饰实际上是溶剂化物（[Ru（bpy）_3]（PF_6）_2·1.5CH_3COCH_3;三角型; P32，a = 13.8133（7）A，c = 11.6523（7）A，Z = 2）。通过溶液介导的平衡，新的修饰被证明是基于成核动力学形成的亚稳（Ostwald）产物。离子去溶剂化后，溶剂化物转变为第二对映体晶体结构（γ型; P3_1，a = 10.3809（4），c = 26.2576（13）A，Z = 3）。后者以前只能通过结晶前的化学拆分获得，而不能直接从外消旋溶液中获得。但是，现在可以通过所谓的“夹带分辨率”方法将新的δ-修饰用于光学分辨率。该实施例强调了相对于晶体工程，动力学控制的溶剂化物结晶和去溶剂化的潜力。

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