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Correction to “Isolation and Structural Characterization of Geminal Di(iodozincio)methane Complexes Stabilized with Nitrogen Ligands”
Journal of the American Chemical Society ( IF 14.4 ) Pub Date : 2021-11-26 , DOI: 10.1021/jacs.1c10680
Yusuke Nishida , Naoki Hosokawa , Masahito Murai , Kazuhiko Takai

The NMR data of TMEDA-CH2(ZnI)23 was reported incorrectly in the paper. The data reported in the original manuscript were for TMEDA-CH3ZnI, which was generated by hydrolysis of 3 in CDCl3. Although the CDCl3 used in this study was distilled and dried over 4 Å molecular sieves, residual HCl or H2O could quench 3. Pure 3 was stable, and no decomposition was observed in the 1H NMR spectra after maintaining the solution of 3 in THF or CH2Cl2 at room temperature for 24 h. With these corrections, the following sentences should be revised as shown: Lines 12–15 of the left column on page 115: Change to “The chemical shift of the active methylene carbon in 3 was −1.51 ppm, compared with −0.55 ppm for that of 1 (both in CDCl3), reflecting electron donation from the TMEDA ligand.” Starting at line 2 from the bottom of the left column on page 115: Remove the sentence, “The singlet 1H NMR resonances for other methylene protons were also found to be absent after the complexes lutidine-CH2(ZnI)22 and TMEDA-CH2(ZnI)23 were kept in CD2Cl2 or CDCl3 at 25 °C for 24 h.16” Starting at line 9 of the right column on page 115: Remove the sentences, “Moreover, when the insoluble white solid was treated with conc. HCl in CDCl3 at 25 °C, evolution of methane gas was observed by 1H NMR analysis (Figure S4). These observations demonstrate the decomposition of gem-di(iodozincio)methane complexes 13 by a Schlenk equilibrium in the solution state.” Page S4 in the Supporting Information (SI): Change the NMR data as follows. 1H NMR (400 MHz, CDCl3): δ −1.51 (s, 2H), 2.58 (s, 8H), 2.60 (m, 24H). 13C NMR (100 MHz, CDCl3): δ −13.4, 47.8, 56.9. Pages S12, S13, and S17 in the SI: Remove Figures S3, S4, and S7 reporting the NMR experiments of 3 conducted in CDCl3. TMEDA-ZnI2 and CH4 shown in Figures S3 and S4 were generated by Schlenk equilibrium or quenching of TMEDA-CH3ZnI, respectively. Because 3 worked as a methylenation reagent, as demonstrated in Scheme 3c, the isolation and purification methods were correct, and the error may have occurred only when 3 was dissolved in CDCl3. No error is present in the NMR data listed in the SI for complexes 1, 2, and 4 as measured in CD2Cl2. The error did not affect the reported yields or data, and the conclusions of this manuscript, i.e. “Isolation and Structural Characterization of Geminal Di(iodozincio)methane” as in the title, remain valid. The authors sincerely apologize for the errors in the NMR data. The Supporting Information is available free of charge at https://pubs.acs.org/doi/10.1021/jacs.1c10680.
  • Experimental details and revised characterization data (PDF)
Experimental details and revised characterization data (PDF) Most electronic Supporting Information files are available without a subscription to ACS Web Editions. Such files may be downloaded by article for research use (if there is a public use license linked to the relevant article, that license may permit other uses). Permission may be obtained from ACS for other uses through requests via the RightsLink permission system: http://pubs.acs.org/page/copyright/permissions.html. This article has not yet been cited by other publications. The Supporting Information is available free of charge at https://pubs.acs.org/doi/10.1021/jacs.1c10680.
  • Experimental details and revised characterization data (PDF)
Experimental details and revised characterization data (PDF) Most electronic Supporting Information files are available without a subscription to ACS Web Editions. Such files may be downloaded by article for research use (if there is a public use license linked to the relevant article, that license may permit other uses). Permission may be obtained from ACS for other uses through requests via the RightsLink permission system: http://pubs.acs.org/page/copyright/permissions.html.


中文翻译:

更正“用氮配体稳定的 Geminal Di(iodozincio)methane 配合物的分离和结构表征”

论文中错误地报告了 TMEDA-CH 2 (ZnI) 2 3的 NMR 数据。原稿中报告的数据是针对 TMEDA-CH 3 ZnI,它是通过3在 CDCl 3 中水解产生的。尽管本研究中使用的 CDCl 3是在 4 Å 分子筛上蒸馏和干燥的,但残留的 HCl 或 H 2 O 可以淬灭3。纯3是稳定的,保持3在THF或CH 2 Cl 2中的溶液后,在1 H NMR谱中没有观察到分解在室温下放置 24 小时。通过这些更正,以下句子应修改如下: 第 115 页左栏第 12-15 行:更改为“ 3 中活性亚甲基碳的化学位移为 -1.51 ppm,相比之下为 -0.55 ppm的1(均在CDCl 3),反射从TMEDA配体电子供给“。从第 115 页左栏底部的第 2 行开始:删除句子,“在配合物二甲基吡啶-CH 2 (ZnI) 2 2和 TMEDA之后,还发现其他亚甲基质子的单线态1 H NMR 共振不存在-CH 2 (ZnI) 2 3保存在CD 2Cl 2或CDCl 3在25°C 下24 小时。16 ” 从第 115 页右栏第 9 行开始:删除句子,“此外,当不溶性白色固体用浓溶液处理时。在 25 °C 的CDCl 3中的HCl,通过1 H NMR 分析观察到甲烷气体的释放(图 S4)。这些观察结果表明的分解宝石-二(iodozincio)甲烷络合物1 - 3通过的Schlenk在溶液状态平衡“。支持信息 (SI) 中的第 S4 页:按如下方式更改 NMR 数据。1 H NMR(400 MHz,CDCl 3):δ -1.51(s,2H),2.58(s,8H),2.60(m,24H)。13C NMR(100 MHz,CDCl 3):δ -13.4、47.8、56.9。SI 中的第 S12、S13 和 S17 页:删除图 S3、S4 和 S7,其中报告了在 CDCl 3 中进行的3的 NMR 实验。图 S3 和 S4 中所示的TMEDA-ZnI 2和 CH 4分别由 TMEDA-CH 3 ZnI的 Schlenk 平衡或淬火产生。由于3作为亚甲基化试剂起作用,如Scheme 3c所示,分离纯化方法是正确的,只有当3溶解在CDCl 3 中时才会出现错误。不存在错误在SI为络合物列出的NMR数据12, 和4在 CD 2 Cl 2 中测量。该错误不影响报告的产量或​​数据,该手稿的结论,即标题中的“ Geminal Di(iodozincio)methane 的分离和结构表征”仍然有效。作者对 NMR 数据中的错误表示诚挚的歉意。支持信息可在 https://pubs.acs.org/doi/10.1021/jacs.1c10680 免费获得。
  • 实验细节和修改后的表征数据 (PDF)
实验细节和修改后的特征数据 (PDF) 大多数电子支持信息文件无需订阅 ACS 网络版本即可获得。此类文件可以按文章下载用于研究用途(如果相关文章有公共使用许可,则该许可可能允许其他用途)。可以通过 RightsLink 许可系统的请求从 ACS 获得许可用于其他用途:http://pubs.acs.org/page/copyright/permissions.html。这篇文章还没有被其他出版物引用。支持信息可在 https://pubs.acs.org/doi/10.1021/jacs.1c10680 免费获得。
  • 实验细节和修改后的表征数据 (PDF)
实验细节和修改后的特征数据 (PDF) 大多数电子支持信息文件无需订阅 ACS 网络版本即可获得。此类文件可以按文章下载用于研究用途(如果相关文章有公共使用许可,则该许可可能允许其他用途)。可以通过 RightsLink 许可系统的请求从 ACS 获得许可用于其他用途:http://pubs.acs.org/page/copyright/permissions.html。
更新日期:2021-12-08
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