Department of Chemistry and Biochemistry , University of California , Santa Barbara , California 93106 , United States.
Inorg Chem. 2018 Jul 16;57(14):8189-8194. doi: 10.1021/acs.inorgchem.8b00672. Epub 2018 Jun 26.
Herein, we report a re-examination of the synthesis and characterization of monolayer-protected Co (SCHCHPh) nanoclusters. These clusters were reportedly formed by the reaction of CoCl with NaBH in the presence of HSCHCHPh and were suggested to contain between 25 and 30 Co atoms. In our hands, however, we found no experimental evidence to support the existence of these large clusters in the reaction mixture. Instead, this reaction results in the relatively clean formation of the cobalt(II) coordination complex [Co(SCHCHPh)Cl] (1). Complex 1 has been fully characterized using a wide variety of techniques, including single-crystal X-ray crystallography, NMR spectroscopy, mass spectrometry, and magnetometry. This complex represents the first example of a thiolate-protected Co(II) T3 supertetrahedral cluster.
在此，我们重新考察了单层保护的 Co(SCHCHPh)纳米团簇的合成与表征。据称，这些团簇是由 CoCl 与 NaBH 在 HSCHCHPh 的存在下反应形成的，并且被认为含有 25 到 30 个 Co 原子。然而，在我们的实验中，我们没有发现支持这些大团簇在反应混合物中存在的实验证据。相反，该反应相对干净地生成了钴(II)配位配合物[Co(SCHCHPh)Cl]（1）。通过使用各种技术，包括单晶 X 射线晶体学、NMR 光谱学、质谱和磁测量法，对配合物 1 进行了充分的表征。该配合物代表了首例硫醇保护的 Co(II)T3 超四面体团簇。
