解密-晶体测试案例26(规则多面体晶体)

DJ_Tokyo

解密-晶体测试案例26(规则多面体晶体)

该晶体是2025年2月27日推文“晶体测试案例26(规则多面体晶体)”所诉案例，如今已发表SCI论文，现解密如下。

最近，同单位某课题组同学委托笔者帮忙测试晶体，含CHNOBr元素的无手性纯有机化合物（2-bromo-9-hydroxy-1,3a-diphenyl-2,9-dihydrocyclopenta[b]chromene-3,3(3aH)-dicarbonitrile[1], CCDC[2]: 2431993,DOI[3]: 10.5517/ccdc.csd.cc2mmpdc），其结构如图1所示（由ChemBioDraw[4]绘制），样品如图2所示，虽然有很多团结成大团的晶簇，但都是由规则的单颗多面体晶体组成，因此从中找一颗干净的单颗晶体即可用于测试。

▲图1 案例结构

▲图2 晶体样品

用真空硅脂（7501高真空硅脂）将该晶体粘在直径与其大小相当的玻璃丝顶端，如图3所示。

▲图3 安装好的晶体

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0.0609 × 0.1661 × 0.2507mm3，如图4‒6所示（由APEX3[5]呈现），最小尺寸不大于另两个任意尺寸的二分之一，是典型的片状（plate）晶体，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

上机测试，钼靶1秒曝光时间测定晶胞，发现衍射点不错，决定收集完整数据，按照10秒曝光时间收集完整数据，大约耗费1个小时，其衍射图如图7所示（由APEX4[6]呈现），共收集到4轮336帧衍射图，总大小为294 MB。

▲图7 衍射图

该晶体在测试过程中发生了滑动，经妥善数据处理后，结构解析和精修结果如图8所示（由Olex2[7]呈现），无AB级警报。

▲图8 解析结果

视频讲解请参阅：

晶体测试案例26(规则多面体晶体)：https://www.bilibili.com/video/BV1smPneKE9H

单晶结构解析练习661(数据还原-晶体滑动-文献案例-氢原子无序)：https://www.bilibili.com/video/BV1n3vFzBEsD

数据下载：

论文PDF+CIF：

链接:https://pan.baidu.com/s/1N1Aos4eXoJyaV90WansZKQ

提取码: kseu

晶体数据：

链接:https://pan.baidu.com/s/1nRcqXVsPp5ZflEIWnrK_vA

提取码: n3ti

参考文献

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声明：本文仅代表个人观点，笔者学识有限，资料整理过程中可能存在疏漏错误，请不吝指正。