具有D_3对称性的M_5L_6型超分子簇的设计、合成与磁性质研究
摘要
近年来,随着材料科学的不断发展进步,人们已经不再满足于只获得具有单一性质和功能的材料,而是更加青睐于能够获得同时具有两种或两种以上性质和功能的材料,如兼具导电性与磁性、磁-光学性、多孔性与磁性、手性与磁性等,特别是自从1997年Rikken和Raupach两位科学家在一种手性顺磁材料中观察到有弱的磁-手二色性(MChD)后,设计具有手性特征的磁性材料,由于具有理论上研究不对称磁各向异性和磁手二色性以及实际中可作为多种材料的潜在应用价值而特别引起人们的兴趣,所以设计兼具奇异手性和磁性的分子材料迅速成为超分子化学最热门的研究领域。但是由于金属和配体之间配位关系的多样化,以及磁相互作用的复杂性,人们对于准确预测配合物结构和磁性质之间的关系还存在很大的困难,到目前为止,仅有少量这样的材料被报导,所以如何对配体和金属离子进行合理的选择与设计,使其按照我们期望的方式进行配位,成为构建此类型材料的关键所在。
本文正是以构建此类兼具手性与磁性的分子材料为研究目标,设计合成了一系列以1,2-二(2-苯并咪唑)乙烯醇为配体的具有D_3对称性的M_5L_6型簇合物,分别对其形态、磁性质以及水热反应条件下形成此类金属簇合物的反应机理进行了研究,并对构-磁关系进行了总结,具体研究结果如下:
1、对现有的具有C_(3h)对称性的五核配合物模型进行改进,首次构建了全新的具有D_3对称性的M_5L_6三螺旋结构模型,并据此模型选择了之前从未被报导过的双苯并咪唑类化合物1,2-二(2-苯并咪唑)乙烯醇为配体,进行配合物的合成。将此平面三齿配体放入设计的模型中,既便于控制配体与金属离子之间的配位方式,得到预期结构的金属配合物,又可有效缩短相邻金属离子之间的距离,使金属离子之间的磁相互作用得到更有效的传递。
2、根据设计的模型,分别用微波和水热方法合成得到了配体及十种M_5L_6型簇合物,所有簇合物均为首次报导。通过红外光谱、紫外光谱、热重-差热图谱、元素分析、ICP及X-射线单晶衍射等方法确定了这10种配合物为同形结构,可由通式M_5L_6·X_nY_(4-n)·mH_2O(X,Y分别代表不同的阴离子)表示,它们都属于单斜晶系,P2_1/c空间群,结构参数上也只有很小的变化,如晶胞参数a,b,c及β的变化范围分别为,13.019(2)～13.330(3)(?),26.132(5)～26.880(2)(?),28.969(2)～29.237(5)(?)和104.976～106.535(9)°,其中单一金属的体系有六种,分别是全镍体系和全钴体系;双金属体系的有四种,分别为镍-铜体系,镍-锌体系,钴-锌体系和铁-锌体系。十种配合物均由一个四价阳离子,四个一价阴离子及溶剂分子构成,其中作为主体结构的四价阳离子[M_5L_6]~(4+)除配合物7外,基本类似,只是其中的金属离子有所替换,而外界阴离子与溶剂分子随金属离子的变换有所不同。在主结构中,六个平面配体上的O原子,按照模型设计,充当桥基连接了五个排布成三角双锥的金属离子,六个配体平均分为三组,组与组之间的夹角近乎垂直,每组中的两个配体近乎平行,平面间的距离为3.3-3.5(?),表明有较强的π-π相互作用。五个金属离子的配位构型也有所不同,分别是位于C_3轴上的两个金属离子采用六配位八面体构型,位于赤道平面的三个金属离子采用四配位四面体构型,整个四价阳离子[M_5L_6]~(4+)具有D_3对称性。10种配合物中,主体结构唯一有所不同的配合物7表现在四价阳离子上还存在一个由苯并咪唑上未参与与五核配位的N原子与Cu~Ⅰ(H_2O)配位。如果不考虑这个一价铜离子,整个配合物的主结构同上述配合物基本类似。此外,配合物的圆二色谱表明配合物在溶液状态下保持了其手性特征,即我们分别从配合物的分子结构和圆二色谱证实了其手性特征确实存在,圆满地完成本课题设计手性金属配合物的第一个目标。
3.发现了罕见的具有金属-有机配位结构的管状簇合物,并对其形态进行了研究。在合成的M_5L_6型金属配合物中,含有金属镍(Ⅱ)的配合物除了阴离子为硝酸根离子时,配合物的形态为颗粒状外,其余配合物均为一端开口,一端封闭的四面体或六面体管状形态,管的长度在250～750μm,管口直径30～70μm,管壁厚度不均,平均壁厚为15μm。体系中镍含量的不同以及是否有其他金属的加入都对配合物管状形态的质量有较大的影响,其中镍-铜混合的配合物的管状物质量最好,在室温下可以稳定存在,且管表面光滑,无裂纹或孔洞,其余配合物所形成的管表面都不同程度的存在裂纹或孔洞。研究发现,反应体系的温度、时间,反应物的pH值等均对产物的形态有影响,结果表明,只有在温度范围为423到448K,反应时间大于92小时且反应物pH值在4到7的范围内,此类含有金属镍的配合物才能形成比较完整的管状形态。改变任一条件,均对配合物的形态有影响。
4、对配合物的变温磁化率曲线进行分析比较后,发现此类M_5L_6型配合物总体表现出反铁磁相互作用,这应该与主结构中较大的M-O-M键角有关,但是对于不同的金属体系,配合物的磁性质存在有较大的差异。对于含有金属镍的体系,当金属为全镍时,四种配合物变温磁化率曲线中xT值随T降低单调减小,且xT值大小类似,表明外界阴离子和溶剂分子的不同对整个体系的反铁磁相互作用没有太大的影响;镍-铜体系,变温磁化率曲线类似于全镍体系,这是由于铜本身也是一种磁性元素且铜离子在体系中所占的百分含量很少,所以对体系整个的磁交换作用改变不大;但是对于镍-锌体系,变温磁化率曲线在低温区表现出弱的铁磁相互作用,进一步的实验证明出现此种作用的温度点在T=8K。我们将这种低温时弱的铁磁相互作用解释为电子自旋的canting效应,这种现象提示我们,在此种含有金属镍的体系中掺杂非磁性金属可以导致配合物磁性质的改变;对于金属为全钴的体系,虽然总体上都表现出反铁磁相互作用,但是xT值随T变化的曲线存在有较大的差别,这是由于外界阴离子和溶剂分子的不同会使主结构中存在一定的差异,再加上Co(Ⅱ)离子的磁各向异性较大所引起的;对于铁-锌体系,虽然整体表现为反铁磁性,但在高温区表现出了弱的铁磁相互作用。这种由于锌掺杂而改变体系磁性质的现象将为人们构筑金属离子簇合物类分子性铁磁体提供新的研究思路。
我们用自旋全矩阵方法对含有Ni_5O_6核的体系进行了理论拟合,根据结构特点定义了三种J值,拟合后所有J值为负,证明体系金属离子之间存在反铁磁相互作用;对配合物4的分子密度泛函理论研究也证明在多重度为3的态中,体系能量最低,此时5个Ni原子中有三个Ni是自旋平行的,而另外两个Ni与它们自旋反平行,表明该磁性分子是反铁磁的。两种理论计算结果均与磁性质实验测量结果相一致。
5、由于在合成过程中所使用配方的不同,除了获得预期具有D_3对称性的金属配合物外,还得到了具有配体1,2-二(2-苯并咪唑)乙烯醇部分结构的化合物,依据这些化合物的结构,我们提出了在此类M_5L_6型金属配合物的水热合成过程中可能发生的反应机理。
Recent years obtaining materials with dual functionalities or multifunctionalities attracts considerable attention,e.g.,conductivity and magnetism,magnetic and optical properties,porosity and magnetism,and chirality and magnetism,etc.Particularly,since magnetochiral dichroism(MChD) effect was observed,the design of molecular materials with interesting chirality and magnetism has become an intense new area of investigation at the forefront of supramolecular chemistry,because these materials are not only of academic interests such as asymmetric magnetic anisotropy,magnetic chirality,and magnetochiral dichroism but also have potential for applications as new devices.However, it still remains difficult to predict structures and magnetic behaviors due to the diversity of coordination and the complicated nature of magnetic interactions.As a consequence few examples of this type of magnet exist.So intelligent ligand design and proper metal centers choice are the main keys to the design of such coordination polymers.
To be interested in this molecular materials and contribute to magneto-structural work on M_5L_6 systems with D_3 symmetry,we report herein the rational design,synthesis, single-crystal structures,configuration,magnetic behaviors and mechanism of the reaction under hydrothermal conditions of the new family of M_5L_6 isomorphous complexes.The main conclusion is as follows:
(ⅰ) On the basis of pentanuclear cluster with C_(3h) symmetry,we constructed a new M_5L_6 cluster model with D_3 symmetry firstly and put a planar tridentate ligand, (Z)-1,2-di(1H-benzo[d]imidazol-2-yl)ethenol,which combines a bridging alkoxide oxygen and benzimidazole nitrogen donors together and has never been reported,in our M_5L_6 model.This rigid ligand was capable of controlling the structure of production and transferring the magnetic interactions effectively between metal ions.
(ⅱ) Based on the model,we synthesized the ligand and ten new complexes under microwave and hydrothermal conditions respectively.These complexes were characterized by IR,UV,TG-DTA,EA,ICP and crystal structure,and analysis revealed that they were isomorphous clusters with the same space group P2_(1/c) and the similar crystal data,as a[13.019(2)～13.330(3)(?)],b[26.132(5)～26.880(2)(?)],c[28.969(2)～29.237(5)(?)], andβ[104.976～106.535(9)°],and can be expressed by M_5L_6·X_nY_(4-n)·mH_2O(X and Y represented different anions).There were six homopentanuclear clusters with Ni~Ⅱand Co~Ⅱand four heteropentanuclear clusters with Ni~Ⅱ-Cu~Ⅱand Cu~Ⅰ,Ni~Ⅱ-Zn~Ⅱ,Co~Ⅱ-Zn~Ⅱand Fe~Ⅱ-Zn~Ⅱ.All of complexes were comprised of a[M_5L_6]~(4+) cation,four univalent anions and solvents except for complex 7.The similar cation constructed by six planar ligands around the M_5O_6 core,which were divided into three roughly parallel pairs with interplane distances in the range 3.3-3.5(?),and each pair was approximatively perpendicular to the others.Five metal ions were in trigonal bipyramidal geometry and displayed two different coordination environments:the two apex metal ions laying on the C_3 axis had octahedral coordinated geometries and the other equatorial metal ions had tetrahedral coordinated geometries.The entire complex cation,therefore,had D_3 symmetry.Complex 7 which was different from other structures put up a linear monovalent copper coordinated by a water and one benzimidazole N.Therefore,ignoring the attached monovalent copper atom, the cation of this complex was the similar to other complexes.The X-ray single crystal diffraction and circular dichroism(CD) spectrum both confirmed the chirality of the complexes,which accorded with our project.
(ⅲ) Tubular metal-organic complexes are very rare.Up to now,only one has been described.In my study,tube morphology can be observed in complexes containing nickel(Ⅱ) ions except for using nickel(Ⅱ) nitrate as reactant.These tubular crystals showed hollow tetragonal or hexahedral prisms and all formed with an open and a closed terminis. The length of the tubes varied from 250 to 750μm and their diameters were in the range of 30-70μm.The wall thickness(ca.15μm on average) varied greatly.Among the complexes,Ni~Ⅱ-Cu~Ⅱand Cu~Ⅰsystem had the best image with glazed surface,and others had crackles or finestras.In order to probe the factors which may affect the formation of the tubular crystals,we varied the length of heating time,temperature and the pH.Tubular crystals can be produced with temperatures varying from 423 to 448 K and heating time longer than 92h with pH between 4 and 7.
(ⅳ) The magnetic behaviors of all these M_5L_6 complexes showed dominant antiferromagnetic interactions,which were consistent with large M-O-M bridge angles. But there were also many differences in their magnetic properties.As for simplex Ni systems,the shape and value of the x_mT versus T plot were similar,so they showed the similar antiferromagnetism though with different aions and solvent molecules;when Cu(Ⅱ) and Cu(Ⅰ)joined,because of their magnetic ions and small quantity,the influence was puny and the magnetic behavior was similar to the simplex Ni systems;but when the nonmagnetic ion Zn(Ⅱ) joined with large proportion,the system exhibited spin-canted antiferromagnetism at low temperature and the critical temperature was at 8K.This phenomenon prompted us that the system doped with nonmagnetic Zn(Ⅱ) ion may change the magnetism of the complexes.As for simplex Co systems,there were obvious differences in magnetic moment,though they had the similar cations.It may be the results of tiny differences between their main structures and the large anisotropy of Co(Ⅱ).The Fe~Ⅱ-Zn~Ⅱsystem had the weak ferromagnetic interactions in the high temperature.These phenomenon that the magnetism of complexes can be changed when the system doped with Zn(Ⅱ) ion may create a new investigative field of molecular-based ferromagnets.
Based on the different distances between Ni(Ⅱ) ions,we defined three exchange parameters(J) in the systems containing Ni_5O_6 core.Best-fit parameters applying the spin matrix method showed all J negative,which confirmed the overall anti-ferromagnetic exchange within these clusters.DFT study also confirmed this conclusion.
(ⅴ) Because of trying different reactive schemes,we obtained other complexes which were composed of the fragment of ligand(Z)-1,2-di(1H-benzoimidazol-2-yl)ethenol besides the M_5L_6 clusters,so we brought forward the possible mechanism of the reaction under hydrothermal conditions.
本文正是以构建此类兼具手性与磁性的分子材料为研究目标,设计合成了一系列以1,2-二(2-苯并咪唑)乙烯醇为配体的具有D_3对称性的M_5L_6型簇合物,分别对其形态、磁性质以及水热反应条件下形成此类金属簇合物的反应机理进行了研究,并对构-磁关系进行了总结,具体研究结果如下:
1、对现有的具有C_(3h)对称性的五核配合物模型进行改进,首次构建了全新的具有D_3对称性的M_5L_6三螺旋结构模型,并据此模型选择了之前从未被报导过的双苯并咪唑类化合物1,2-二(2-苯并咪唑)乙烯醇为配体,进行配合物的合成。将此平面三齿配体放入设计的模型中,既便于控制配体与金属离子之间的配位方式,得到预期结构的金属配合物,又可有效缩短相邻金属离子之间的距离,使金属离子之间的磁相互作用得到更有效的传递。
2、根据设计的模型,分别用微波和水热方法合成得到了配体及十种M_5L_6型簇合物,所有簇合物均为首次报导。通过红外光谱、紫外光谱、热重-差热图谱、元素分析、ICP及X-射线单晶衍射等方法确定了这10种配合物为同形结构,可由通式M_5L_6·X_nY_(4-n)·mH_2O(X,Y分别代表不同的阴离子)表示,它们都属于单斜晶系,P2_1/c空间群,结构参数上也只有很小的变化,如晶胞参数a,b,c及β的变化范围分别为,13.019(2)～13.330(3)(?),26.132(5)～26.880(2)(?),28.969(2)～29.237(5)(?)和104.976～106.535(9)°,其中单一金属的体系有六种,分别是全镍体系和全钴体系;双金属体系的有四种,分别为镍-铜体系,镍-锌体系,钴-锌体系和铁-锌体系。十种配合物均由一个四价阳离子,四个一价阴离子及溶剂分子构成,其中作为主体结构的四价阳离子[M_5L_6]~(4+)除配合物7外,基本类似,只是其中的金属离子有所替换,而外界阴离子与溶剂分子随金属离子的变换有所不同。在主结构中,六个平面配体上的O原子,按照模型设计,充当桥基连接了五个排布成三角双锥的金属离子,六个配体平均分为三组,组与组之间的夹角近乎垂直,每组中的两个配体近乎平行,平面间的距离为3.3-3.5(?),表明有较强的π-π相互作用。五个金属离子的配位构型也有所不同,分别是位于C_3轴上的两个金属离子采用六配位八面体构型,位于赤道平面的三个金属离子采用四配位四面体构型,整个四价阳离子[M_5L_6]~(4+)具有D_3对称性。10种配合物中,主体结构唯一有所不同的配合物7表现在四价阳离子上还存在一个由苯并咪唑上未参与与五核配位的N原子与Cu~Ⅰ(H_2O)配位。如果不考虑这个一价铜离子,整个配合物的主结构同上述配合物基本类似。此外,配合物的圆二色谱表明配合物在溶液状态下保持了其手性特征,即我们分别从配合物的分子结构和圆二色谱证实了其手性特征确实存在,圆满地完成本课题设计手性金属配合物的第一个目标。
3.发现了罕见的具有金属-有机配位结构的管状簇合物,并对其形态进行了研究。在合成的M_5L_6型金属配合物中,含有金属镍(Ⅱ)的配合物除了阴离子为硝酸根离子时,配合物的形态为颗粒状外,其余配合物均为一端开口,一端封闭的四面体或六面体管状形态,管的长度在250～750μm,管口直径30～70μm,管壁厚度不均,平均壁厚为15μm。体系中镍含量的不同以及是否有其他金属的加入都对配合物管状形态的质量有较大的影响,其中镍-铜混合的配合物的管状物质量最好,在室温下可以稳定存在,且管表面光滑,无裂纹或孔洞,其余配合物所形成的管表面都不同程度的存在裂纹或孔洞。研究发现,反应体系的温度、时间,反应物的pH值等均对产物的形态有影响,结果表明,只有在温度范围为423到448K,反应时间大于92小时且反应物pH值在4到7的范围内,此类含有金属镍的配合物才能形成比较完整的管状形态。改变任一条件,均对配合物的形态有影响。
4、对配合物的变温磁化率曲线进行分析比较后,发现此类M_5L_6型配合物总体表现出反铁磁相互作用,这应该与主结构中较大的M-O-M键角有关,但是对于不同的金属体系,配合物的磁性质存在有较大的差异。对于含有金属镍的体系,当金属为全镍时,四种配合物变温磁化率曲线中xT值随T降低单调减小,且xT值大小类似,表明外界阴离子和溶剂分子的不同对整个体系的反铁磁相互作用没有太大的影响;镍-铜体系,变温磁化率曲线类似于全镍体系,这是由于铜本身也是一种磁性元素且铜离子在体系中所占的百分含量很少,所以对体系整个的磁交换作用改变不大;但是对于镍-锌体系,变温磁化率曲线在低温区表现出弱的铁磁相互作用,进一步的实验证明出现此种作用的温度点在T=8K。我们将这种低温时弱的铁磁相互作用解释为电子自旋的canting效应,这种现象提示我们,在此种含有金属镍的体系中掺杂非磁性金属可以导致配合物磁性质的改变;对于金属为全钴的体系,虽然总体上都表现出反铁磁相互作用,但是xT值随T变化的曲线存在有较大的差别,这是由于外界阴离子和溶剂分子的不同会使主结构中存在一定的差异,再加上Co(Ⅱ)离子的磁各向异性较大所引起的;对于铁-锌体系,虽然整体表现为反铁磁性,但在高温区表现出了弱的铁磁相互作用。这种由于锌掺杂而改变体系磁性质的现象将为人们构筑金属离子簇合物类分子性铁磁体提供新的研究思路。
我们用自旋全矩阵方法对含有Ni_5O_6核的体系进行了理论拟合,根据结构特点定义了三种J值,拟合后所有J值为负,证明体系金属离子之间存在反铁磁相互作用;对配合物4的分子密度泛函理论研究也证明在多重度为3的态中,体系能量最低,此时5个Ni原子中有三个Ni是自旋平行的,而另外两个Ni与它们自旋反平行,表明该磁性分子是反铁磁的。两种理论计算结果均与磁性质实验测量结果相一致。
5、由于在合成过程中所使用配方的不同,除了获得预期具有D_3对称性的金属配合物外,还得到了具有配体1,2-二(2-苯并咪唑)乙烯醇部分结构的化合物,依据这些化合物的结构,我们提出了在此类M_5L_6型金属配合物的水热合成过程中可能发生的反应机理。
Recent years obtaining materials with dual functionalities or multifunctionalities attracts considerable attention,e.g.,conductivity and magnetism,magnetic and optical properties,porosity and magnetism,and chirality and magnetism,etc.Particularly,since magnetochiral dichroism(MChD) effect was observed,the design of molecular materials with interesting chirality and magnetism has become an intense new area of investigation at the forefront of supramolecular chemistry,because these materials are not only of academic interests such as asymmetric magnetic anisotropy,magnetic chirality,and magnetochiral dichroism but also have potential for applications as new devices.However, it still remains difficult to predict structures and magnetic behaviors due to the diversity of coordination and the complicated nature of magnetic interactions.As a consequence few examples of this type of magnet exist.So intelligent ligand design and proper metal centers choice are the main keys to the design of such coordination polymers.
To be interested in this molecular materials and contribute to magneto-structural work on M_5L_6 systems with D_3 symmetry,we report herein the rational design,synthesis, single-crystal structures,configuration,magnetic behaviors and mechanism of the reaction under hydrothermal conditions of the new family of M_5L_6 isomorphous complexes.The main conclusion is as follows:
(ⅰ) On the basis of pentanuclear cluster with C_(3h) symmetry,we constructed a new M_5L_6 cluster model with D_3 symmetry firstly and put a planar tridentate ligand, (Z)-1,2-di(1H-benzo[d]imidazol-2-yl)ethenol,which combines a bridging alkoxide oxygen and benzimidazole nitrogen donors together and has never been reported,in our M_5L_6 model.This rigid ligand was capable of controlling the structure of production and transferring the magnetic interactions effectively between metal ions.
(ⅱ) Based on the model,we synthesized the ligand and ten new complexes under microwave and hydrothermal conditions respectively.These complexes were characterized by IR,UV,TG-DTA,EA,ICP and crystal structure,and analysis revealed that they were isomorphous clusters with the same space group P2_(1/c) and the similar crystal data,as a[13.019(2)～13.330(3)(?)],b[26.132(5)～26.880(2)(?)],c[28.969(2)～29.237(5)(?)], andβ[104.976～106.535(9)°],and can be expressed by M_5L_6·X_nY_(4-n)·mH_2O(X and Y represented different anions).There were six homopentanuclear clusters with Ni~Ⅱand Co~Ⅱand four heteropentanuclear clusters with Ni~Ⅱ-Cu~Ⅱand Cu~Ⅰ,Ni~Ⅱ-Zn~Ⅱ,Co~Ⅱ-Zn~Ⅱand Fe~Ⅱ-Zn~Ⅱ.All of complexes were comprised of a[M_5L_6]~(4+) cation,four univalent anions and solvents except for complex 7.The similar cation constructed by six planar ligands around the M_5O_6 core,which were divided into three roughly parallel pairs with interplane distances in the range 3.3-3.5(?),and each pair was approximatively perpendicular to the others.Five metal ions were in trigonal bipyramidal geometry and displayed two different coordination environments:the two apex metal ions laying on the C_3 axis had octahedral coordinated geometries and the other equatorial metal ions had tetrahedral coordinated geometries.The entire complex cation,therefore,had D_3 symmetry.Complex 7 which was different from other structures put up a linear monovalent copper coordinated by a water and one benzimidazole N.Therefore,ignoring the attached monovalent copper atom, the cation of this complex was the similar to other complexes.The X-ray single crystal diffraction and circular dichroism(CD) spectrum both confirmed the chirality of the complexes,which accorded with our project.
(ⅲ) Tubular metal-organic complexes are very rare.Up to now,only one has been described.In my study,tube morphology can be observed in complexes containing nickel(Ⅱ) ions except for using nickel(Ⅱ) nitrate as reactant.These tubular crystals showed hollow tetragonal or hexahedral prisms and all formed with an open and a closed terminis. The length of the tubes varied from 250 to 750μm and their diameters were in the range of 30-70μm.The wall thickness(ca.15μm on average) varied greatly.Among the complexes,Ni~Ⅱ-Cu~Ⅱand Cu~Ⅰsystem had the best image with glazed surface,and others had crackles or finestras.In order to probe the factors which may affect the formation of the tubular crystals,we varied the length of heating time,temperature and the pH.Tubular crystals can be produced with temperatures varying from 423 to 448 K and heating time longer than 92h with pH between 4 and 7.
(ⅳ) The magnetic behaviors of all these M_5L_6 complexes showed dominant antiferromagnetic interactions,which were consistent with large M-O-M bridge angles. But there were also many differences in their magnetic properties.As for simplex Ni systems,the shape and value of the x_mT versus T plot were similar,so they showed the similar antiferromagnetism though with different aions and solvent molecules;when Cu(Ⅱ) and Cu(Ⅰ)joined,because of their magnetic ions and small quantity,the influence was puny and the magnetic behavior was similar to the simplex Ni systems;but when the nonmagnetic ion Zn(Ⅱ) joined with large proportion,the system exhibited spin-canted antiferromagnetism at low temperature and the critical temperature was at 8K.This phenomenon prompted us that the system doped with nonmagnetic Zn(Ⅱ) ion may change the magnetism of the complexes.As for simplex Co systems,there were obvious differences in magnetic moment,though they had the similar cations.It may be the results of tiny differences between their main structures and the large anisotropy of Co(Ⅱ).The Fe~Ⅱ-Zn~Ⅱsystem had the weak ferromagnetic interactions in the high temperature.These phenomenon that the magnetism of complexes can be changed when the system doped with Zn(Ⅱ) ion may create a new investigative field of molecular-based ferromagnets.
Based on the different distances between Ni(Ⅱ) ions,we defined three exchange parameters(J) in the systems containing Ni_5O_6 core.Best-fit parameters applying the spin matrix method showed all J negative,which confirmed the overall anti-ferromagnetic exchange within these clusters.DFT study also confirmed this conclusion.
(ⅴ) Because of trying different reactive schemes,we obtained other complexes which were composed of the fragment of ligand(Z)-1,2-di(1H-benzoimidazol-2-yl)ethenol besides the M_5L_6 clusters,so we brought forward the possible mechanism of the reaction under hydrothermal conditions.
引文
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