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.

中文翻译：

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叔丁基二氯膦：晶体结构及其对超甲硅烷基钠的反应性

的晶体t氯丁烷2通过在 80 °C/0.150 mbar 下的短程升华获得。结构测定t氯丁烷2是基于 X 射线粉末数据。测量在 173 K 至 rt 的温度范围内进行。在 173 K 时，X 射线粉末图案被指定为斜方相，在 213 K 时被指定为塑性结晶立方相。我们进一步研究了t氯丁烷2朝向Na(thf)2[硅t布3] 在环境温度下。反应为t氯丁烷2具有两个当量的 Na(thf)2[硅t布3] 一起给予t布3SiCl 尚不为人知的磷二钠2[PtBu]通过氯-钠交换。娜的身份2[PtBu] 得到证实31P NMR 光谱及其存在通过其与甲醇的质子化和随后形成t丁苯酚2。