Abstract
Crystals of tBuPCl2 were obtained by a short-path sublimation at 80 °C/0.150 mbar. The structure determination of tBuPCl2 was based on X-ray powder data. The measurements were carried out in a temperature range from 173 K to r. t. At 173 K the X-ray powder pattern has been assigned to an orthorhombic phase, and that at 213 K to a plastic-crystalline, cubic phase. We further investigated the reactivity of tBuPCl2 towards Na(thf)2[SitBu3] at ambient temperature. The reaction of tBuPCl2 with two equivalents of Na(thf)2[SitBu3] gave together with tBu3SiCl the yet unknown phosphanediide Na2[PtBu] by a chlorine-sodium exchange. The identity of Na2[PtBu] was confirmed by 31P NMR spectroscopy and its existence was unambiguously demonstrated by its protonation with methanol and the consequent formation of tBuPH2.
Acknowledgments
M. B. wishes to thank the Fonds der Chemischen Industrie (FCI) for a Kekulé Ph.D. grant.
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Research ethics: Not applicable.
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Author contributions: The authors have accepted responsibility for the entire content of this manuscript and approved its submission.
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Competing interests: The authors state no conflict of interest.
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Research funding: None declared.
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Data availability: Not applicable.
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