解密-晶体测试案例11(弱衍射晶体)

DJ_Tokyo

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解密-晶体测试案例11(弱衍射晶体)

该晶体是2024年12月10日推文“晶体测试案例11(弱衍射晶体)”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让笔者帮忙测晶体，送来了2颗晶体，含CHO元素非手性纯有机化合物（diethyl (4Z,6E)-8-phenyl-15-(p-tolyl)-14-(p-tolylethynyl)-12,13-dihydro-11H-1(1,6)-indena-2(1,4)-benzenacyclooctaphane-4,6-diene-12,12-dicarboxylate[1], CCDC[2]: 2467462,2499981, DOI[3]: 10.5517/ccdc.csd.cc2ntlkn, 10.5517/ccdc.csd.cc2pxfkm），其结构如图1所示（由ChemBioDraw[4]绘制），样品如图2所示。

▲图1 案例结构

▲图2 送来的2颗晶体

右边那颗晶体是层叠堆积生长的金字塔状，显然无法用于测试，左边这颗也有点多颗堆积生长的迹象，对左边这颗晶体进行切割，笔者的操作是用针灸针（或用粉刺针）将其戳碎，然后从碎片中寻找合适的晶体，如图3所示。

▲图3 戳碎的晶体碎片

从碎片中选择了图3红色箭头所指的那颗，将其用真空硅脂粘在与其大小一致的玻璃丝顶端，如图4所示。

▲图4 安装在玻璃丝顶端的待测晶体

在晶体对心时测量并记录下晶体尺寸为0.199 × 0.227 × 0.329 mm3，如图5‒7所示（由APEX3[5]呈现）。（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”和“晶体尺寸的测量：https://www.bilibili.com/video/BV1hM4y1J71o”。）

▲图5 晶体尺寸测量

▲图6 晶体尺寸测量

▲图7 晶体尺寸测量

首先测晶胞，用钼靶1秒曝光时间，发现衍射很弱，如图8所示。

▲图8 钼靶1秒曝光时间衍射情况

于是正式测试的时候换用更强的铜靶作为光源，曝光时间设为10秒，其衍射图如图9所示（由APEX4[6]呈现）。

▲图9 铜靶10秒曝光时间衍射情况

最终数据处理结果如图10所示（由Olex2[7]呈现），无AB级警报，不过晶体质量的确不太好，所以R因子有点高。

▲图10 最终数据结果

视频讲解请参阅：

单晶结构解析练习707(文献案例-数据还原)：https://www.bilibili.com/video/BV1wWkdBYEUe

数据下载：

论文PDF+CIF：

链接:https://pan.baidu.com/s/19Y0UdDcquhKnHrxkr9PGJw?pwd=jbee

提取码: jbee

晶体数据：

链接:https://pan.baidu.com/s/1g61daRSiDT03w5L9lh5oPw?pwd=p3e3

提取码: p3e3

参考文献

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