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Syntheses and Molecular Structures of Novel Alkali Metal Tetraorganyl-cyclopentaphosphanides and Tetraorganyltetraphosphane-1,4-diides

机译:新型碱金属四有机基-环五膦酸酯和四有机基四膦-1,4-二酰亚胺的合成及分子结构

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The reaction of sodium with RPC1_2 and PC1_3 (12:4:1) in THF gives Na[cyclo-(P_5R_4)] [R=iPr (1),Ph (2)],while four equivalents of RPC1_2 [R=Ph,2,4,6-Me_3C_6H_2 (Mes),tBu] react with ten equivalents of sodium sand or elemental potassium in re-fluxing THF to yield the compounds [Na_2(THF)_5(P_4Ph_4)] (3),[Na_2(THF)_4(P_4Mes_4)] (4),and [Na_2(THF)_4(P_4tBu_4)] (5),or the potassium salt [K_2(THF)_6(P_4Mes_4)] (6).Recrystallizing 6 from 1,4-dioxane/pentane (1:3) also led to {K(L)_2(_2(K(L))_6-(P_4Mes_4_)4·0.5THF)_(ident to) (L=1,4-dioxane) (7).In the solid state,compounds 3-6 exist as isolated ion-contact complexes,in which the P_4 chain of the (P_4R_4)~(2-) ligand has a syn arrangement,while a polymeric helical arrangement was observed for 7.A minor product,[(K(pmdeta)(HP_3Mes_3))_2(K_2-(P_4Mes_4))]·0.25hexane (8),was isolated from the reaction of MesPCl_2 and K (1:2.5).Compound 8 contains the first structurally characterized example of a triphosphanide anion,(HP_3Mes_3)~-,besides K_2(P_4Mes-4).
机译:钠与RPC1_2和PC1_3(12:4:1)在THF中的反应得到Na [cyclo-(P_5R_4)] [R = iPr(1),Ph(2)],而四当量的RPC1_2 [R = Ph, 2,4,6-Me_3C_6H_2(Mes),tBu]与十当量的钠砂或元素钾反应,使THF回流,得到化合物[Na_2(THF)_5(P_4Ph_4)](3),[Na_2(THF) )_4(P_4Mes_4)](4)和[Na_2(THF)_4(P_4tBu_4)](5)或钾盐[K_2(THF)_6(P_4Mes_4)](6)。从1,4-重结晶6。二恶烷/戊烷(1:3)也导致{K(L)_2(_2(K(L))_ 6-(P_4Mes_4_)4·0.5THF)_(与)相同(L = 1,4-二恶烷)( 7)。在固态下,化合物3-6以孤立的离子接触络合物的形式存在,其中(P_4R_4)〜(2-)配体的P_4链具有顺式排列,而对于7则观察到聚合物螺旋排列从MesPCl_2与K(1:2.5)的反应中分离出次要产物[[K(pmdeta)(HP_3Mes_3))_ 2(K_2-(P_4Mes_4))·0.25己烷(8)。化合物8含有K_2(P_4)以外的三phosph阴离子(HP_3Mes_3)〜-的第一个结构特征实例Mes-4)。

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