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首页> 外文期刊>Chemistry: A European journal >A Nonanuclear Copper(II) Polyoxometalate Assembled Around a mu-1,1,1,3,3,3-Azido Ligand and Its Parent Tetranuclear Complex
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A Nonanuclear Copper(II) Polyoxometalate Assembled Around a mu-1,1,1,3,3,3-Azido Ligand and Its Parent Tetranuclear Complex

机译：围绕mu-1,1,1,1,3,3,3-叠氮基配体及其母体四核配合物组装的非核多金属铜（II）

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摘要

Reaction of Cu~(II), [gamma-SiW_(10)O_(36)]~(8-),and N_3 affords three azido polyoxotungstate complexes.Two of them have been characterized by single-crystal X-ray diffraction.Complex KNaCs_(10)[{gamma-SiW_(10)O_(36)Cu_2(H_2O)-(N_3)_2}_2]centre dot 26H_2O (1) is obtained as crystals in few hours after addition of CsCl.This linear tetranuclear Cu~(II) complex consists in two [gamma-SiW_(10)O_(36)Cu_2-(H_2O)(N_3)_2]~(6-) units connected through two W=O bridges.When the filtrate is left to stand for one night,a new complex is obtained.From both elemental analysis and IR spectroscopy,it has been postulated that this compound could be formulated K_(1.5)Cs_(5.5)[SiW_(10)O_(37)-Cu_2(H_2O)_2(N_3)]cenmtre dot 14H_2O (la),showing the loss of one azido ligand per poly-oxometalate unit.Finally,when no cesium salt is added to the reaction medium,the nonanuclear complex K_(12)Na_7[{SiW_8O_(31)Cu_3(OH)(H_2O)_2(N_3)}_3-(N_3)]centre dot 24H_2O (2) is obtained after three days.Compound 2 crystallizes in the R3c space group and consists in three (Cu_3) units related by a C_3 axis passing through the exceptional mu-l,1,1,3,3,3-azido bridging ligand.Each trinuclear Cu~(II) unit is embedded in the [gamma-SiW_8O_(31)]~(10-) ligand,an unprecedented tetravacant polyoxometalate,showing that partial decomposition of the [y-SiW_(10)O_(36)]~(8-) precursor occurs with time in such experimental conditions.Magnetically,complex 1 behaves as two isolated {Cu_2(mu_(1.1)-N_3)_2) pairs in which the metal centers are strongly ferromagnet-ically coupled (J= + 224cm~(-1),g = 2.20),the coupling through the W=O bridges being negligible.The magnetic behavior of complex 2 has also been studied.Relatively weak ferromagnetic couplings (J_1 = +1.0 cm~(-1),J_2 = + 20.0 cm~(-1),g = 2.17) have been found inside the {Cu_3} units,while the intertri-meric magnetic interactions occurring through the hexadentate azido ligand have been found to be antiferromag-netic (J_3 = - 5.4cm~(-1)) and ferromagnetic (J_4 = + 1.3 cm~(-1)) with respect to the end-to-end and end-on azido-bridged Cu~(II) pairs,respectively.
机译：Cu〜（II），[γ-SiW_（10）O_（36）]〜（8-）与N_3的反应生成了3个叠氮基多氧钨酸盐络合物，其中两个已通过单晶X射线衍射表征。加入CsCl后数小时即可获得KNaCs_（10）[{γ-SiW_（10）O_（36）Cu_2（H_2O）-（N_3）_2} _2]中心点26H_2O（1）的晶体。该线性四核Cu 〜（II）络合物由两个通过两个W = O桥连接的[γ-SiW_（10）O_（36）Cu_2-（H_2O）（N_3）_2]〜（6-）单元组成。当滤液静置时从元素分析和红外光谱两方面推测，该化合物可以配制成K_（1.5）Cs_（5.5）[SiW_（10）O_（37）-Cu_2（H_2O） _2（N_3）]中心点14H_2O（la），表明每个多金属氧酸盐单元损失一个叠氮基配体。最后，当不向反应介质中添加铯盐时，非核络合物K_（12）Na_7 [{SiW_8O_（ 31天后三天，获得了Cu_3（OH）（H_2O）_2（N_3）} _ 3-（N_3）]中心点24H_2O（2）。 R3c空间群由三个（Cu_3）单元组成，三个C_3轴相关联，它们穿过特殊的mu-1,1,1,3,3,3-叠氮基桥联配体。每个三核Cu〜（II）单元都嵌入[γ-SiW_（8O_（31）]〜（10-）配体，前所未有的四空位多金属氧酸盐，表明[y-SiW_（10）O_（36）]〜（8-）前体随时间发生部分分解磁性地，络合物1表现为两个独立的{Cu_2（mu_（1.1）-N_3）_2）对，其中金属中心强铁磁耦合（J = + 224cm〜（-1），g = 2.20）还研究了配合物2的磁性。相对弱的铁磁耦合（J_1 = +1.0 cm〜（-1），J_2 = + 20.0 cm〜（-1）， g = 2.17）被发现在{Cu_3}单元内部，而通过六齿叠氮基配体发生的三聚体间的磁性相互作用被发现是反铁磁性的（J_3 =-5.4cm〜（-1））和铁磁性的（ J_4 = + 1.3厘米〜 （-1））分别关于端对端和端对叠氮基桥接的Cu〜（II）对。

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