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首页> 外文期刊>Russian Journal of Coordination Chemistry >New n Ligand N,N,N,N',N',N'-Hexaallylethylenediaminium (L~(2+)): Synthesis and Crystal Structures of LBr2 · 2H2O and Its Cuprocomplexes L[Cu~(II)(Br_(0.45)Cl_(3.55))], L[Cu4(Br_(4.55)Cl_(1.45))], and L[Cu4Br6]
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New n Ligand N,N,N,N',N',N'-Hexaallylethylenediaminium (L~(2+)): Synthesis and Crystal Structures of LBr2 · 2H2O and Its Cuprocomplexes L[Cu~(II)(Br_(0.45)Cl_(3.55))], L[Cu4(Br_(4.55)Cl_(1.45))], and L[Cu4Br6]

机译:新的n配体N,N,N,N',N',N'-六烯丙基乙烯二铵(L〜(2+)):LBr2·2H2O及其铜配合物L [Cu〜(II)(Br_(0.45 )Cl_(3.55))],L [Cu4(Br_(4.55)Cl_(1.45))]和L [Cu4Br6]

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摘要

The alkylation of ethylenediamine with allyl bromide in the presence of a fourfold (with respect to ethylenediamine) molar amount of NaHCO3 in acetone with an ethanol admixture (15 : 1) affords LBr2 · 2H2O (I), where L~(2+) is the N,N,N,N',N',N'-hexaallylethylenediaminium cation. Single crystals of complexes L[Cu~(II)(Br_(0.45)Cl_(3.55))] (II), L[ Cu_4~I (Br_(4.55)Cl_(1.45))] (III), and L[Cu4 Br6] (IV) are prepared by ac electrochemical synthesis from an ethanolic solution of LBr2 · 2H2O, CuCl2 · 2H2O (or CuBr2) at copper wire electrodes. The crystal structures of compounds I-IV are determined by X-ray diffraction analysis. The crystals of complex I are mon-oclinic: space group P2_1, a = 8.544(3), b = 10.404(3), c = 13.350(4) A, β = 97.29(3)°, V = 1177.2(6) A~3, Z=2. The bromine anions in compound I are bonded to the L~(2+) cations and water molecules through hydrogen contacts (E)H···Br (E = O, C) of 2.57(3)-2.86(3) A. The crystals of compounds II-IV are triclinic: space group P1. For II: a = 8.762(4), b = 9.163(4), c = 16.500(6) A, α = 95.62(4)°, β = 96.39(4)°, γ= 111.46(4)°, V = 1211.4(9) A~3, Z= 2; for III: a = 9.074(4), b = 9.435(4), c = 9.829(5) A, α = 116.12(4)°, β = 104.14(4)°, γ = 100.22(4)°, V = 692.3(6) A~3, Z= 1; for IV isostructural III: a = 9.084(4), b = 9.404(4), c = 9.869(4) A, α = 116.31(3)°, β = 104.00(3)°, γ = 100.37(3)°, V= 692.1(5) A , Z= 1. Unlike the isolated tetrahedral CuX_4~(2-) anion in structure II, an original chain anion (Cu4X_6~(2-) )_n is observed in the structures of π complexes III and IV.
机译:乙二胺与烯丙基溴在丙酮中以乙醇混合物(15:1)在丙酮中有四倍(相对于乙二胺)摩尔量的NaHCO3烷基化,得到LBr2·2H2O(I),其中L〜(2+)为N,N,N,N′,N′,N′-六烯丙基乙烯二铵阳离子。配合物L [Cu〜(II)(Br_(0.45)Cl_(3.55))](II),L [Cu_4〜I(Br_(4.55)Cl_(1.45))](III)和L [Cu4通过在铜丝电极上由LBr2·2H2O,CuCl2·2H2O(或CuBr2)的乙醇溶液通过交流电化学合成来制备[Br6](IV)。化合物I-IV的晶体结构通过X射线衍射分析确定。配合物I的晶体是单斜晶的:空间群P2_1 / n,a = 8.544(3),b = 10.404(3),c = 13.350(4)A,β= 97.29(3)°,V = 1177.2( 6)A〜3,Z = 2。化合物I中的溴阴离子通过2.57(3)-2.86(3)A的氢接触(E)H··Br(E = O,C)与L〜(2+)阳离子和水分子键合。化合物II-IV的晶体是三斜晶的:空间群P1。对于II:a = 8.762(4),b = 9.163(4),c = 16.500(6)A,α= 95.62(4)°,β= 96.39(4)°,γ= 111.46(4)°,V = 1211.4(9)A〜3,Z = 2;对于III:a = 9.074(4),b = 9.435(4),c = 9.829(5)A,α= 116.12(4)°,β= 104.14(4)°,γ= 100.22(4)°,V = 692.3(6)A〜3,Z = 1;对于IV等结构III:a = 9.084(4),b = 9.404(4),c = 9.869(4)A,α= 116.31(3)°,β= 104.00(3)°,γ= 100.37(3)° ,V = 692.1(5)A,Z =1。与结构II中分离的四面体CuX_4〜(2-)阴离子不同,在π配合物III的结构中观察到原始链状阴离子(Cu4X_6〜(2-))_n和IV。

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