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首页> 外文期刊>Journal of chemical crystallography >A Facile Synthesis and Crystallographic Analysis of Seven Trityl Phosphorus Compounds and Two Nickel(II) Phosphine Side-Products
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A Facile Synthesis and Crystallographic Analysis of Seven Trityl Phosphorus Compounds and Two Nickel(II) Phosphine Side-Products

机译：七个三苯甲基磷化合物和两个镍（II）膦膦副产物的简便合成和晶体学分析

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摘要

The syntheses and X-ray analyses of triphenylmethyl (trityl=Tr) phosphorus compounds are reported and the structural similarities, differences and 31 P chemical shifts compared. A series of seven trityl-substituted phosphorus-containing compounds have been characterized by single crystal X-ray diffraction. Ph3CPPh2, 1, a bulky P(III) compound crystallizes in the triclinic space group P (1) over bar, a = 7.5624(6) angstrom, b = 9.5470(8) angstrom, c = 16.9722(14) angstrom, alpha = 83.4720(10)degrees, beta = 80.541(2)degrees, gamma = 68.1580(10)degrees, the borane complex of 1, 2, Ph3CPPh2(BH3) crystallizes as monoclinic colorless crystals, P2(1)/c, a = 10.0972(12) angstrom, b = 9.6955(12) angstrom, c = 25.197(3) angstrom, beta = 90.258(2)degrees. The analogous methyl substituted, 3, Ph3CPMe2(BH3) is monoclinic, C-2/c, a = 15.628(3) angstrom, b = 12.770(3) angstrom, c = 18.406(4) angstrom, beta = 103.968(3)degrees. Compounds 4-7 are trityl substituted P(V) compounds: Ph3CP(Ph)(O)(OH), 4, crystallizes in the triclinic space group P (1) over bar, a = 8.9847(18) angstrom, b = 9.7443(19) angstrom, c = 12.786(3) angstrom, alpha = 72.045(3)degrees, beta = 72.031(3)degrees, gamma = 78.769(3)degrees. Esterification of 4 affords TrCP(O)(Ph)OBn 5, space group, P2(1)/c, a = 7.9196(5) angstrom, b = 31.701(2) A, c = 19.8062(13) angstrom, b = 99.7750(10)degrees. A phosphonate diester was also characterized, Ph3CP(O)(OEt) 2, 6, triclinic, P (1) over bar, a = 7.9521(17) angstrom, b = 9.2205(19) angstrom, c = 14.471(3) angstrom, alpha = 85.906(4)degrees, beta = 83.031(4)degrees, gamma = 68.283(4)degrees. Treatment of the trityl H-phosphinic acid, Ph3CPO2H2, with elemental selenium yields yellow crystals of 7, [Ph3CP(O)(OH)Se](2), P2(1)/c, a = 9.0603(4) angstrom, b = 22.3652(11) angstrom, c = 16.9134(7) angstrom, beta = 107.035(2)degrees. In our efforts to isolate a nickel-phosphine complex, two Ni(II) complexes were crystallographically analyzed, [Ni(OP(H)Ph-2)(6)](2)BF(4)(-)8 and 9. Complex 8 with an uncoordinatedBF(4)(-) ion crystallizes as yellow orthorhombic crystals, Pbca, a = 18.8247(12) angstrom, b = 18.5518(12) angstrom, c = 21.0976(14) A, while crystals of 9 are trigonal, R (3) over barc, a = b = 13.1545(12) angstrom, c = 68.461(9) angstrom.
机译：报告了三苯甲基（三苯甲基= Tr）磷化合物的合成和X射线分析，并比较了结构相似性，差异和31 P化学位移。通过单晶X射线衍射表征了一系列七个三苯甲基取代的含磷化合物。 Ph3CPPh2，1，一个庞大的P（III）化合物在三栏式空间群P（1）上结晶，a = 7.5624（6）埃，b = 9.5470（8）埃，c = 16.9722（14）埃，alpha = 83.4720（10）度，β= 80.541（2）度，γ= 68.1580（10）度，1,2，Ph3CPPh2（BH3）的硼烷配合物结晶为单斜无色晶体，P2（1）/ c，a = 10.0972 （12）埃，b = 9.6955（12）埃，c = 25.197（3）埃，β= 90.258（2）度。类似的甲基取代的3，Ph3CPMe2（BH3）是单斜晶的，C-2 / c，a = 15.628（3）埃，b = 12.770（3）埃，c = 18.406（4）埃，beta = 103.968（3）度。化合物4-7是三苯甲基取代的P（V）化合物：Ph3CP（Ph）（O）（OH），4，在三边形空间群P（1）中结晶成bar，a = 8.9847（18）埃，b = 9.7443 （19）埃，c = 12.786（3）埃，alpha = 72.045（3）度，beta = 72.031（3）度，γ= 78.769（3）度。酯化4得到TrCP（O）（Ph）OBn 5，空间群，P2（1）/ c，a = 7.9196（5）埃，b = 31.701（2）A，c = 19.8062（13）埃，b = 99.7750（10）度还表征了膦酸酯二酯，Ph3CP（O）（OEt）2、6，三斜晶，P（1）超过bar，a = 7.9521（17）埃，b = 9.2205（19）埃，c = 14.471（3）埃，alpha = 85.906（4）度，beta = 83.031（4）度，gamma = 68.283（4）度。用元素硒处理三苯甲基H-次膦酸Ph3CPO2H2产生黄色晶体7，[Ph3CP（O）（OH）Se]（2），P2（1）/ c，a = 9.0603（4）埃，b = 22.3652（11）埃，c = 16.9134（7）埃，beta = 107.035（2）度。在我们努力分离镍-膦配合物的过程中，对两个Ni（II）配合物进行了晶体学分析，[Ni（OP（H）Ph-2）（6）]（2）BF（4）（-）8和9。具有未配位BF（4）（-）离子的配合物8结晶为黄色正交晶体，Pbca，a = 18.8247（12）埃，b = 18.5518（12）埃，c = 21.0976（14）A，而9的晶体是三角晶体，R（3）在barc上，a = b = 13.1545（12）埃，c = 68.461（9）埃。

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