文章中关于晶体测试解析与精修的描述示例5

数据来源：J. Am. Chem. Soc. 2020, 142, 15246−15251.

DOI：10.1021/jacs.0c07083

CCDC：1959113，2009659

以下内容来自上述文章的支撑文献：

蓝色中文注释以及图片均由笔者添加，如有不对或不妥之处，请读者朋友指正，谢谢！

Single-Crystal Characteristics.

Single-crystal growth – ternary solvent diffusion. (单晶培养方法：三元溶剂扩散（液相扩散）) A solution prepared from ~1 mg NFA in 0.3 mL CHCl3 was transferred into an NMR tube. Around 0.2 mL of CH2Cl2 was carefully layered on top of the CHCl3 solution, followed by carefully layering acetone or hexanes on top. The CH2Cl2 portion plays an important role as a buffer layer to create a gradient of solubility, which facilitates slow growth of crystals and suppresses the rapid precipitation of solids. The NMR tube was then sealed and left standing for a few days (3-7 days) until the color of the solution faded away. (培养单晶的容器：核磁管。三元溶剂扩散：将约1毫克样品溶于0.3毫升氯仿中并置于核磁管底部，在其上铺上0.2毫升二氯甲烷，随后在顶部铺上丙酮或正己烷，从而形成三元溶剂扩散体系。其中中间的二氯甲烷溶剂层充当缓冲层，其作用是产生溶解度梯度，这有助于晶体缓慢生长（晶体生长速度慢则质量佳）并抑制固体的快速沉淀) Y6, CH1007 and IT-4F were grown using this method.

Single-crystal growth – vapor diffusion. (单晶培养方法：气相扩散) This method was used for growing crystals of NFAs based on linear π-cores. A solution prepared from ~1 mg NFA in ~0.5 mL toluene or CHCl3 was transferred into a 4 mL vial, which was capped with a piece of aluminum foil with a hole punched using a 24G needle in the middle. The 4 mL vial was then placed in a 20 mL vial containing ~3 mL CH3CN, acetone or MeOH. The 20 mL vial was then tightly sealed, and left standing for a few days (2-4 days) to give small crystal clusters. (将约1毫克样品溶于0.5毫升甲苯或氯仿中并转移至4毫升样品瓶中，瓶口用铝箔盖上，并插一个针头（用于气相扩散），然后将该4毫升样品瓶放入含有约3毫升乙腈、丙酮或甲醇的20毫升样品瓶中，并将20毫升样品瓶密封形成封闭空间，4毫升和20毫升样品瓶中的溶剂在该封闭体系中通过枕头的小孔扩散至彼此溶剂体系中，静置待其扩散生长晶体。)ITIC, 4TIC, STIC and 6TIC-4F were grown using this method.

Single-crystal X-ray diffraction of Y6. A black lustrous prism with a bronze colored shimmer (晶体形状（shape）和颜色（color）), measuring 0.40 × 0.20 × 0.07 mm3 (晶体物理尺寸) was mounted on a loop with oil (晶体安装方式：晶体用油包裹并安装在loop环上). Data was collected at -173 °C (数据采集温度（低温）) on a Bruker APEX II single-crystal X-ray diffractometer (单晶衍射仪：布鲁克AEPX II), Mo-radiation (辐射光源：钼靶). The crystals were stable under oil for only 5 minutes (单晶稳定性：在油的包裹下仅能稳定5分钟). Crystal-to-detector distance was 40 mm (晶体与探测器之间的距离) and exposure time was 120 seconds (曝光时间) per frame for all sets. The scan width was 0.5° (扫描步长). Data collection was 99.1% complete to 25° in θ (数据完整度). A total of 29810 reflections were collected covering the indices, -28<=h<=28, -68<=k<=68, -17<=l<=17, with Rint = 0.2471. Indexing and unit cell refinement indicated a C-centered monoclinic lattice. The space group was found to be C2/c (No.15).

Single-crystal X-ray diffraction of CH1007. A black piece, measuring 0.11 × 0.15 × 0.32 mm3 was mounted on a loop with oil. Data was collected at -173 °C on a Bruker APEX II single-crystal X-ray diffractometer, Mo-radiation. Crystal-to-detector distance was 40 mm and exposure time was 60 seconds per frame for all sets. The scan width was 1°. Data collection was 94.3% complete to 25° in θ. A total of 31724 unique reflections were collected covering the indices, -13<=h<=13, -22<=k<=22, -30<=l<=30, with Rint = 0.2200. Indexing and unit cell refinement indicated a triclinic lattice. The space group was found to be Pī (No. 2).