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首页> 外文期刊>Crystal growth & design >The Phenomenon of Conglomerate Crystallization. Part 57. Control of the Crystallization Behavior by the Choice of the Counter Ion. Part 9. The Stereochemistry and Crystallization Architecture of [(3,2,3-tet)Co(N_3)_2]X (X = Cl(I), Br(II), I(III), NO_
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The Phenomenon of Conglomerate Crystallization. Part 57. Control of the Crystallization Behavior by the Choice of the Counter Ion. Part 9. The Stereochemistry and Crystallization Architecture of [(3,2,3-tet)Co(N_3)_2]X (X = Cl(I), Br(II), I(III), NO_

机译：砾岩结晶现象。第57部分：通过选择反离子来控制结晶行为。第9部分。[（3,2,3-tet）Co（N_3）_2] X（X = Cl（I），Br（II），I（III），NO_的立体化学和结晶结构

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Compounds of composition of [(3,2,3-tet)Co(N_3)_2]X(X = Cl(I), Br(II), I(III), NO_3(IV), and PF_6(V)) were prepared, and their crystal structures were determined at 295 and 120 K. Unlike a previous study by this group, in which we reported [Saha, M. K.; Bernal, I. Inorg. Chem. Commun. 2002, accepted for publication] a change of space group (P2_1 to P2_1) upon cooling a cis-bis-diazido compound of Co(III), all the compounds described here retain their space groups upon cooling from 295 to 120 K. There are measurable changes in cell constants but no larger than what one normally expects. Details of the syntheses and of the crystallographic determinations are given below. A full description of the changes in stereochemistry of the [(3,2,3-tet)Co(N_3)_2]~+ counteranions, are detailed quantitatively, and superposition diagrams of the cations have been included to illustrate the changes in bond angles and torsional angles concomitant with the changes in anions and thus producing channel frameworks of different architecture. As expected, variations in bond lengths are minute, if at all, statistically vaild. Compounds (I)-(IV) are racemates at all temperatures, while (V) is a conglomerate (space group P6_1 at 295 and 120 K), neatly illustrating the counteranion dependence of the phenomenon of conglomerate crystallization. Water molecules occupy channels in the framework of compound (I), which can be dehydrated and rehydrated without destruction of the crystal lattice.
机译：[（3,2,3-tet）Co（N_3）_2] X（X = Cl（I），Br（II），I（III），NO_3（IV）和PF_6（V）的组成的化合物制备了它们的晶体结构，并在295和120 K下确定了它们的晶体结构。与该小组先前的研究不同，在该研究中我们报道了[Saha，MK; Bernal，I。Inorg。化学公社[2002年，接受出版]冷却Co（III）的顺式-双-重氮基化合物时，空间基团的变化（从P2_1 / n到P2_1），此处所述的所有化合物在从295 K冷却至120 K时仍保留其空间基团。单元常数有可测量的变化，但不大于正常预期的变化。合成和晶体学测定的细节在下面给出。定量详细描述了[（3,2,3-tet）Co（N_3）_2]〜+阴离子的立体化学变化，并包括了阳离子的叠加图以说明键角的变化。和扭转角与阴离子的变化相伴，从而产生不同结构的通道骨架。不出所料，键长的变化在统计上是微小的，即使有的话也是如此。化合物（I）-（IV）在所有温度下均为外消旋物，而（V）为团聚体（295和120 K时的空间群P6_1），清楚地说明了团聚体结晶现象的抗衡离子依赖性。水分子占据化合物（I）骨架中的通道，可以在不破坏晶格的情况下进行脱水和再水化。

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