晶体测试案例39(薄片晶体)

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晶体测试案例39(薄片晶体)

案例来源：CCDC[1] 2443608. DOI[2]: 10.5517/ccdc.csd.cc2n0s2k.

案例结构为2-氯-1-甲基-1H-苯并咪唑（CAS: 1849-02-1），如图1所示（由ChemBioDraw[3]绘制）。

▲图1 案例结构

晶体培养方法为单一溶剂挥发法，溶剂为甲苯（CAS: 108-88-3），容器为试管，敞口挥发（参阅视频“培养单晶之过滤-挥发法：https://www.bilibili.com/video/BV1mkdWYZEYJ”）。

取样品约50毫克，加入2毫升甲苯，超声溶解，未溶解完全，用注射器+过滤头过滤至试管中，敞口挥发，在有溶剂的情况下未观察到结晶，溶剂挥发干后，发现有片状晶体，如图2所示。

▲图2 试管底部的片状晶体

用刮勺将其捞出，至于载玻片上用二甲基硅油（CAS: 9006-65-9）覆盖，在显微镜下观察，如图3所示。

▲图3 显微镜下的晶体

从中切割挑选表面干净（无小晶体或固体杂质附着）、无裂痕的晶体用于测试。

其晶体尺寸经测量（参阅推文“布鲁克D8 VENTURE测量晶体尺寸操作步骤”或视频“APEX3 D8 Venture对心时晶体尺寸的测量：https://www.bilibili.com/video/BV1Cq4y1d7S5”“晶体尺寸的测量：https://www.bilibili.com/video/BV1hM4y1J71o”）为0.0575 × 0.3859 × 0.7485mm3，如图4‒6所示（由APEX3[4]呈现），一个尺寸很小，另两个尺寸很大，可描述为片状（plate）晶体，最小的尺寸为厚度，参阅视频“晶体尺寸和晶癖描述需保持一致：https://www.bilibili.com/video/BV1yb421B72r”。

▲图4 晶体尺寸测量

▲图5 晶体尺寸测量

▲图6 晶体尺寸测量

用钼靶测试，发现衍射还不错，曝光时间设置为2秒，花费10分钟测得完整数据（3轮共284帧衍射照片，总大小为215 MB），其衍射图如图7所示（由APEX4[5]呈现）。

▲图7 衍射图

最终经数据还原解析后结果如图8（由Olex2[6]呈现）所示，无AB级警报（验证报告由PLATON[7]呈现）。

▲图8 最终结果

相关视频：

单晶结构解析练习557(数据还原)：https://www.bilibili.com/video/BV12boHYQEuk

数据下载：

链接: https://pan.baidu.com/s/1oYi57CZczb6iEKLvryMm5g

提取码: 4a29

参考文献

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