结晶溶剂不同得到不同结构案例1

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结晶溶剂不同得到不同结构案例1

案例来源：CCDC [1]: 2484843 vs. 2518298.Chem. Commun. 2026, 62, 3807–3810. DOI [2]: 10.1039/d5cc06726j.

如图1所示（由ChemBioDraw [3]绘制），利用配体前体H2P-Nm-Ph（N2,N2''-bis((diisopropylphosphanyl)methyl)-[1,1':3',1''-terphenyl]-2,2''-diamine）与2当量氢化钾（KH, potassiumhydride, CAS: 7693-26-7）在四氢呋喃 [4]（THF, tetrahydrofuran, CAS: 109-99-9, CCDC: 1116822–1116823 [4a], 1116824–1116825 [4b]）中室温下反应得到配体钾盐K2P-Nm-Ph，该配体钾盐与四(四氢呋喃)三碘化镧(III) [5]（LaI3(THF)4, CCDC: 1251841 [5a], 2044769 [5b], 2340266 [5c], 2339540 [5d]）在四氢呋喃中室温下反应得到固体产物，该固体产物用正己烷 [6]（C6H14, n-hexane,CAS: 110-54-3, CCDC: 103189）和苯 [7]（（C6H6,benzene, CAS: 71-43-2, CCDC: 1108749–1108750 [7a], 1108751 [7b], 1108752 [7c], 1108753 [7d], 1108754 [7e], 1108755–1108756(C6D6,deuterated benzene, CAS: 1076-43-3) [7f], 1108757–1108759 [7g], 298305–298307 [7h], 682617 [7i], 757059–757061 [7j], 725244 [k], 1454032 [7l], 1423904 [7m], 1579553 [7n], 1579564 [7n], 1581798 [7n], 1581824 [7n], 1843296 [7o], 1843297 [7p], 1913527 [7q], 2201163 [7r]）混合溶剂作为结晶溶剂，得到的是二聚体结构[(η1:η1:η6:η1:η1-P-Nm-Ph)La(μ-I)]2·2C6H6（CCDC: 2484843），而当使用正己烷和四氢呋喃作为结晶溶剂时，得到的则是单核配合物[(η1:η1:η6:η1:η1-P-Nm-Ph)LaI(THF)]（CCDC:2518298）。

▲图1 反应示意图

相关视频和晶体数据：

单晶结构解析练习767(文献案例-数据还原-无序处理)：https://www.bilibili.com/video/BV13uZFB8Evx

单晶结构解析练习768(文献案例-数据还原-无序处理)：https://www.bilibili.com/video/BV1tR9zB4EJh

论文PDF+CIF：

链接:https://pan.baidu.com/s/1dsJdJjng3Za-Rvcz7xGxNA?pwd=23ci

提取码: 23ci

晶体数据（CCDC: 2484843）：

链接:https://pan.baidu.com/s/17X5SaB5vjMSsrsuQXMnj8Q?pwd=v88d

提取码: v88d

晶体数据（CCDC: 2518298）：

链接:https://pan.baidu.com/s/14_FnTjQmgkW_cRvpGX0sGw?pwd=ghrq

提取码: ghrq

参考文献

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