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31P NMR spectroscopy. In a flame-dried sealed NMR tube, trichloride 2 was afforded in a pure form at the initial stage, however, 2 was proved to be partly converted to oxide 3 even in keeping the solution in the sealed NMR tube for 12 h with the ratio of 2 to 3 of 94:6. When the sealed NMR tube containing pure trichloride (prepared as described above) was opened in the glove box, of which moisture level is <1 ppm, the ratio of 2 to 3 became 92:8 after 12 h. We suggest that trichloride 2 is a primary product of this reaction, which is too moisture sensitive to isolate in a pure form. We thank the reviewer for this suggestion.
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