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CrCl 3 (thf) 3 is a common starting material in the synthesis of organometallic and coordination compounds of Cr. Deposited as an irregular solid with no possibility of recrystallization, it is not a purity guaranteed chemical, causing problems in some cases. In this work, we disclose a well-defined form of the THF adduct of CrCl 3 ([CrCl 2 (μ-Cl)(thf) 2 ] 2 ), a crystalline solid, that enables structure determination by X-ray crystallography. The EA data and XRD pattern of the bulk agreed with the revealed structure. Moreover, its preparation procedure is facile: evacuation of CrCl 3 ·6H 2 O at 100 °C, treatment with 6 equivalents of Me 3 SiCl in a minimal amount of THF, and crystallization from CH 2 Cl 2 . The ethylene tetramerization catalyst [iPrN{P(C 6 H 4 - p -Si(nBu) 3 ) 2 } 2 CrCl 2 ] + [B(C 6 F 5 ) 4 ] - prepared using well-defined [CrCl 2 (μ-Cl)(thf) 2 ] 2 as a starting material exhibited a reliably high activity (6600 kg/g-Cr/h; 1-octene selectivity at 40 °C, 75%), while that of the one prepared using the impure CrCl 3 (thf) 3 was inconsistent and relatively low (~3000 kg/g-Cr/h). By using well-defined [CrCl 2 (μ-Cl)(thf) 2 ] 2 as a Cr source, single crystals of [(CH 3 CN) 4 CrCl 2 ] + [B(C 6 F 5 ) 4 ] - and [{Et(Cl)Al(N(iPr) 2 ) 2 }Cr(μ-Cl)] 2 were obtained, allowing structure determination by X-ray crystallography, which had been unsuccessful when the previously known CrCl 3 (thf) 3 was used as the Cr source.

Replacement of the Common Chromium Source CrCl3(thf)3 with Well-Defined [CrCl2(μ-Cl)(thf)2]2