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An unpredictable reaction of tBu _2PHO·BCl _3 in the presence of water

机译:水存在下tBu _2PHO·BCl _3的不可预测的反应

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When a benzene solution of tBu _2PHO·BCl _3 was exposed to air at room temperature, the phosphonium chloride [tBu _2PH _2]Cl was formed together with di-tert-butylphosphinic acid, tBu _2PO(OH). X-ray quality crystals of the hydrochloride [tBu _2PH _2]Cl·HCl were obtained from the reaction solution at room temperature. The hydrochloride [tBu _2PH _2]Cl·HCl crystallizes in the monoclinic space group P2 _1/m, a = 6.3012(7) ?, b = 6.8970(10) ?, c = 14.5011(15) ?, β = 99.376(9)°, V = 621.79(13) ? ~3, Z = 2, d _(calcd) = g cm- ~3 1.165; R1 = 0.0510, wR2 = 0.1503 for 1,129 reflections with I > 2σ(I). The crystal was a non-merohedral twin with a contribution of 0.353(7) of the minor component. The structure is composed of discrete di-t-butylphosphonium cations and Cl anions. Both are located on a crystallographic mirror plane and are connected by P-H...Cl hydrogen bonds.
机译:当室温下将tBu _2PHO·BCl _3的苯溶液暴露于空气中时,氯化di [tBu _2PH _2] Cl与二叔丁基次膦酸tBu _2PO(OH)一起形成。在室温下从反应溶液中获得了盐酸盐[tBu _2PH _2] Cl·HCl的X射线晶体。盐酸盐[tBu _2PH _2] Cl·HCl在单斜空间群P2 _1 / m中结晶,a = 6.3012(7)α,b = 6.8970(10)α,c = 14.5011(15)α,β= 99.376(9 )°,V = 621.79(13)? 〜3,Z = 2,d_(计算)= g cm-〜3 1.165;对于I>2σ(I)的1,129次反射,R1 = 0.0510,wR2 = 0.1503。晶体是非中间面孪晶,占次要成分的0.353(7)。该结构由离散的二叔丁基phosph阳离子和Cl阴离子组成。两者都位于晶体镜面上,并且通过P-H ... Cl氢键连接。

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