配合物[Cd（1,3-BDC）（L）（H2O）2]·H2O的水热合成、晶体结构和荧光性质

利用水热方法制备了一个新的过渡金属镉配合物[Cd(1,3-BDC)(L)(H2O)2]·H2O(1,3-H2BDC=间苯二甲酸,L=2-(3-吡啶基)-1H-苯并咪唑),并通过元素分析、红外光谱和X-射线单晶衍射方法确定了该配合物的晶体结构.结构分析表明该配合物属于单斜晶系,P21/c空间群,晶胞参数a=1.016 41(6)nm,b=2.088 42(12)nm,c=1.001 38(6)nm,β=106.336 0(10)°,V=2.039 8(2)nm3,Z=4,R1=0.020 7,wR2=0.494.配合物中CdⅡ离子与L配体的1个吡啶N原子、1,3-BDC的4个氧原子和2个配位水的O原子配位,形成七配位的扭曲十面体结构.配体1,3-BDC的桥连相邻的CdⅡ离子形成一维聚合物链,相邻链间通过氢键和π…π作用形成三维超分子网络,并对该配合物的热稳定性和荧光性质进行了研究.     

铈配合物[Ce（4-aba）3（4-abaH）（phen）2]·H2O的合成与晶体结构

采用普通溶液法合成了单核铈配合物[Ce(4-aba)3(4-abaH)(phen)2]·H2O(4-abaH=对氨基苯甲酸,phen=1,10-邻菲罗啉)。X射线单晶衍射结果表明:该配合物晶体属单斜晶系,P21/c空间群,晶胞参数:a=1.8896(4)nm,b=1.9755(4)nm,c=1.3200(3)nm,β=97.235(2)°,V=4.8880(18)nm3,Mr=1064.06,Dc=1.446 g·cm-3,Z=4,μ=0.996 mm-1。中心铈离子的配位环境为变形的三帽三棱柱体。配合物存在着π-π堆积及丰富的氢键,将配合物扩展为三维超分子结构。     

新型双核配位聚合物Ni2（A`B`T`C`）（phen）2（H2O）4·4H2O的合成及其晶体结构

以A`B`T`C`(2,2’,3,3’-偶氮苯四甲酸)和Phen(邻啡啰啉)为配体,采用溶剂挥发法合成了一种新型双核配位聚合物Ni2(A`B`T`C`)(phen)2(H2O)4.4H2O(1),其结构经X-射线单晶衍射和元素分析表征。1属三斜晶系,空间群P-1,晶胞参数a=9.432(11),b=10.697(12),c=10.751(12),α=87.946(17)°,β=67.756(15)°,γ=76.085(16)°,V=972.6843,Z=12,Dc=4.740 mg.cm-3,μ=4.039 mm-1,F(000)=1 364,R1=0.042 5,ωR2=0.132 9。1中Ni(Ⅱ)与A`B`T`C中的两个羧基氧原子,两个H2O中的两个氧原子和phen中的两个氮原子配位,形成一个畸变的八面体几何构型。Ni(Ⅱ)经配体A`B`T`C桥联形成一维链,链与链之间又通过氢键堆积成三维超分子结构。     

新型单核Ni（Ⅱ）配合物{[Ni（phen）（H2O）4]·（1,5-nds）·H2O}的合成及其晶体结构

以1,5-萘二磺酸钠和1,10-邻菲罗啉为配体,Ni(Ⅱ)为中心离子,采用蒸发溶剂法,在去离子水中合成了一个新型的单核Ni(Ⅱ)配合物{[Ni(phen)(H2O)4]·(1,5-nds)·H2O(1),phen=1,10-邻菲罗啉,1,5-nds=1,5-萘二磺酸根离子},其结构经IR,元素分析和X-射线单晶衍射表征。1属单斜晶系,空间群C2/c,晶胞参数a=20.590 9(18),b=12.435 0(11),c=12.539 0(12),β=124.652(2)°,Z=4,V=2 641.1(4)3。在1的分子结构中,中心离子Ni(Ⅱ)与phen和四个水分子配位,呈八面体构型;1,5-nds没有配位,起平衡电荷作用。     

混合配体配合物[Cd2(phen)4(bmal)2]·3H2O的合成与晶体结构研究

A novel binucleus mixed-ligand[Cd₂(phen)₄(bmal)₂]·3H₂O (phen=phenanthroline; bmal=benzylmalonic acid radical) has been synthesized by the reaction of phen and bmal with cadmium(Ⅱ) salt. X-ray crystal structure analysis was carried out to determine the crystal structure of the title complex. The crystal of the title complex belongs to monoclinic system with space group P2₁/c, a=1.119 1(8) nm, b=2.480 5(17) nm, c=1.063 4(8) nm, β=142.042(12)°, Z=4, V=2.887(3) nm³, D_c=1.613 g·cm^-3, R₁=0.046 2, wR₂=0.115 6, F(000)=1 424. One carboxyl of bmal is coordinated to Cd(1) with monodentate form, the others are coordinated to Cd(2) with bidentate form. The complexes form a 1-D chain structure bridged by hydrogen bonds that formed by uncoordinated water and oxygen atom of carboxyl group in bmal, the 2-D network structure was formed by π-π interaction of neighbouring phen. CCDC: 257080.     

环状二核铜配合物[Cu(nphth)(phen)(H2O)]2·2H2O的水热合成与晶体结构

在水热反应条件下,合成了一个新配合物,[Cu(nphth)(phen)(H₂O)]₂·2H₂O(nphth=3-硝基邻苯二甲酸阴离子,phen=邻菲 咯啉),经元素分析、红外、热重、单晶衍射表征了配合物。该配合物为单斜晶系,空间群P2₁/n,结构参数：a=0.999 8(1) nm,b=1.044 5(1) nm,c=1.820 6(1) nm,β=91.423(1)°,V=1.900 7(2) nm³,Z=2,R=0.039 4,wR=0.096 5。结构分析表明,配合物为分立环状二核结构,并通过分子间氢键和π-π作用扩展为二维超分子网络结构。     

一种新奇的d-f异双核配合物[Fe(phen)3]2[FeCe(tiron)3]·6H2O的水热合成、晶体结构和磁性

硝酸铁,硝酸铈,邻菲咯啉(phen)和钛铁试剂(Tiron)通过水热方法合成了一种d-f异双核配合物 [Fe(phen)₃]₂[FeCe(tiron)₃]·6H₂O,tiron=C₆H₂O₈S₂。X-射线单晶衍射分析表明,晶体属立方晶系,P2₁3空间群,晶胞参数为：a=2.194 09(4) nm,V=10.562 4(3) nm³,Z=4,F(000)=4 648,R₁=0.045 1,wR₂=0.107 7,S=1.072。在具有C₃对称性的[FeCe(tiron)₃]^6-单元中,Fe(Ⅲ)与6个酚氧配位形成一个反三棱柱配位多面体,Ce(Ⅲ)则与3个桥联的酚氧μ₂-O和3个磺酸基的氧形成另一个与FeO₆共用底面的反三棱柱配位多面体CeO₆。配阳离子通过phen-phen之间的π-π相互作用和与配阴离子间的静电引力等作用组装成一种三角梅状准主/客体型的超分子。在2～300 K温度范围内测试了配合物的变温磁化率,结果表明, Ce(Ⅲ)-Fe(Ⅲ)之间存在典型的反铁磁性相互作用。     

配合物[Sm(o-MOBA)3(phen)·H2O]2·4H2O的合成与晶体结构

The title complex [Sm(o-MOBA)₃(phen)·H₂O]₂·4H₂O has been synthesized by the reaction of SmCl₃·6H₂O with o-methoxybenzoic acid and 1,10-phenanthroline in 1∶3∶1 molar ratio. The crystal structure was determined by X-ray single crystal diffraction. The crystal belongs to triclinic system, space group P1 with a=1.203(10) nm, b=1.293(10) nm, c=1.306(11) nm, α=64.50(10)°, β=81.93(10)°, γ=74.81(10)°. The molecular structure shows that the Sm³⁺ ion coordinates to nine atoms. The carboxylate groups are bonded to the samarium ion in three modes: monodentate, bidentate chelating, tridentate chelating-bridging. CCDC: 603740.     

[Ni(dien)2]2[Mn(NCS)6]·H2O的合成、晶体结构

The crystal of [Ni(dien)₂]₂[Mn(NCS)₆]·H₂O was synthesized and the structure of its single crystal was determined by X-ray diffraction. The crystal is monoclinic system, space group P2₁/c with a=16.544(3),b=15.137(2), c=17.334(3)?, β=99.90(1)°, V=4276.3(12)?³, Z=4, D_c=1.479g·cm^-3, M_r=951.55, F(000)=1998, μ=1.489mm^-1, R=0.0399, R_w=0.0958. IR was also determined.     

吡啶-2，3，5，6-四甲酸镉配合物[Cd(H2PTA)(H2O)3]·3H2O的合成与晶体结构

吡啶羧酸是一类非常有趣、灵活多变的配体,它能与过渡金属离子和稀土金属离子配位形成稳定的配合物,而且配位方式不拘一格.     

二维超分子氢键网络：光致发光配合物[Cu(HIm)(PPh3)2I]的合成与晶体结构

A new photoluminescence supramolecular compound [Cu(HIm)(PPh₃)₂I] was synthesized and characterized by single crystal X-ray diffraction, elemental analysis, as well as IR, UV-Vis absorption and luminescence spectrometry. It crystallizes in monoclinic system, space group P2₁/n with a=1.3335(14) nm, b=1.310 3(9) nm, c=2.154 4(16) nm, α=90.00°, β=101.130(10)°, γ=90.00°, V=3.694(5) nm³, Z=4, D_c=1.408 Mg·m^-3. The single crystal structure indicates that the 2D supramolecular network structure is established by intermolecular weak N-H…I and C-H…I hydrogen-bonding interactions. The N-H…I is responsible for the conformation of one-dimensional zigzag chains and the C-H…I connects these chains to form two-dimensional supramolecular hydrogen-bonding network. At room temperature in the solid state, the complex is photoluminescent with an emission peak maximum at 460 nm, upon excitation at 330 nm. The emission is assigned to the metal-perturbed intraligand (PPh₃) in nature. CCDC: 228743.     

酰胺氮桥联双核钴(Ⅲ)配合物[Co2(bpmb)2(CN)2]·H2O的合成、分子结构和超分子组装

合成了1个酰胺氮桥联的双核钴(Ⅲ)配合物[Co2(bpmb)2(CN)2].H2O(bpmb2-=1,2-bis(pyridine-2-carboxamido)-4-methylbenze-nate)(1),并通过X-射线单晶衍射分析表征其结构特征。结果表明:吡啶甲酰胺配体H2bpmb的甲酰胺氮原子脱去氢原子形成带两个负电荷的扭曲的四配位螯合配体bpmb2-。1个钴(Ⅲ)离子与2个吡啶氮原子,2个bpmb2-配体上的桥联酰胺氮原子和2个氰基碳原子配位得到六配位、变形的八面体CoN4C2;另1个钴(Ⅲ)离子与2个吡啶氮原子,配体bpmb2-上的2个未桥联甲酰胺氮原子和2个桥联的甲酰胺氮原子六配位,形成扭曲的八面体CoN6配位构型。[Co2(bpmb)2(CN)2]单元通过自由水分子和氰基氮原子和甲酰胺氧原子之间O-H…N和O-H…O氢键形成锯齿型链状超分子亚结构,这些链状亚结构通过π-π相互作用连接起来形成网状的超分子结构。     

配合物[Co(phen)2(m-chlorobenzoic acid)2·(H2O)]·(H2O)2的水热合成、晶体结构电化学分析

The title complex has been synthesized with m-chlorobenzoic acid, 1,10-phenanthroline and cobalt perchlorate anhydrous in the solvent mixture of water and methanol. Crystal data for this complex: triclinic, space group P1, a=0.870 7(3) nm, b=1.284 4(4) nm, c=1.692 9(5) nm; α=75.430(5)°, β=77.562(5)°, γ=86.346(5)°, V=1.789 4(9) nm³, D_c=1.456 g·cm^-3, Z=2, F(000)=806. Final GooF=1.065, R₁=0.068 4, wR₂=0.127 5. The crystal stru-cture shows that the Cobaly ion is coordinated with four nitrogen atoms from two 1,10-phenanthroline molecules and two oxygen atoms from one m-chlorobenzoic acid molecule and one water molecule respectively, forming a distorted octahedral coordination geometry. The cyclic voltametric behavior of the complex is also reported. CCDC: 619087.     

配合物[Cu(PTA)(phen)2]·(PTA)·(H2O)4的合成、晶体结构及电化学性质

The title complex has been synthesized by using terephthalic acid (PTA), 1,10-phenanthroline (phen) and copper monohydrate. It crystallizes in monoclinic space group C2/c with a=2.959 0(2) nm, b=1.466 4(10) nm, c=1.764 3(12) nm, β=105.593(11)°, V=7.372(9) nm³, Dc=1.489 g·cm^-3, Z=8, F(000)=3 416, R₁=0.043 6, wR₂= 0.151 9. The crystal structure shows that the copper atom is coordinated with four nitrogen atoms from two phens and one oxygen atom from one terephthalic acid, forming a distorted square-pyramid coordination geometry. The cyclic voltametric behavior of the complex is also reported. CCDC: 277047.     

配合物[Cd(m-nitrobenzoic acid)2(phen)2]·(H2O)2的合成、晶体结构及电化学性质

在乙醇和水的混合溶剂中以间硝基苯甲酸(m-nitrobenzoic acid)、邻菲咯啉(phen)为原料合成了一个新的配合物[Cd(m-nitrobenzoic acid)₂(phen)₂]·(H₂O)₂,该配合物晶体属三斜晶系,空间群P1。配合物中镉原子与2个phen的4个N原子和2个间硝基苯甲酸根的3个羧基氧原子配位形成七配位的五角双锥结构。电化学性质研究表明：标题配合物     

一维异核配合物[KNd(bta)2(H2O)6]·H2O的水热合成，晶体结构和荧光性质

以双四唑胺(H₂bta)、NdCl₃·6H₂O、KOH为原料,用水热法合成了1个一维异核的Nd³⁺配合物[KNd(bta)₂(H₂O)₆]·H₂O。通过X-射线单晶衍射、元素分析、红外光谱对该配合物进行了结构表征。该化合物属于单斜晶系,P2₁/m空间群。每个Nd³⁺与2个来自bta^2-离子的4个氮原子和5个水分子形成了1个盖帽的四方双锥,通过bta^2-和水分子桥联配体把Nd³⁺和K⁺连接成一维链状结构,链与链之间通过O-H…N和N-H…O氢键作用形成三维超分子结构。紫外吸收光谱和荧光光谱表征结果显示该配合物的水溶液在292和412 nm表现出双四唑胺的特征吸收峰和荧光发射特征峰。     

配合物[Mn(2,2′-bipy)(H2O)4]·(m-phth)的水热合成和晶体结构

A mononuclear manganese complex [Mn(2,2′-bipy)(H₂O)₄]·(m-phth) (2,2′-bipy=2,2′-bipyridine, m-phth=isophthalate) has been synthesized by hydrothermal methods. The crystal structure was determined by single-crystal X-ray diffraction. The crystal is of orthorhombic, space group Pnna with a=0.766 8(8) nm, b=2.050 2(2) nm, c=1.247 0(13) nm, V=1.960 4(4) nm³, Z=4, M_r=447.30, D_c=1.376 g·cm^-3, μ=0.722 mm^-1, F(000)=924, R_int=0.027 0, R=0.028 0 and wR=0.075 5. In the crystal the manganese atom is six-coordinated by two nitrogen atoms from 2,2′-bipyradine and four oxygen atoms from water molecules, completing an octahedral coordination geometry. The isophthalate molecules are included in the lattice and connected to Mn(2,2′-bipy)(H₂O)₄ by hydrogen bonding interactions to form a three-dimensional supramolecular structure. CCDC:286965.     

配合物｛[Ni（tyr）2（4,4’-bpt）]·H2O｝·H2O的合成及晶体结构

本文以3,5-二(4-吡啶基)-1,2,4-三唑和酪氨酸为混合配体,利用水热法合成了一个单核镍配合物{[Ni(tyr)2(4,4’-bpt)].H2O}.H2O(1)(其中4,4’-bpt=3,5-二(4-吡啶基)-1,2,4-三唑,Htyr=L-酪氨酸)并利用元素分析、红外光谱和X射线单晶衍射法对其结构进行了表征。结果表明,配合物属于单斜晶系,P21空间群,a=6.0720(12),b=14.083(3),c=17.609(4),β=92.18(3)°,V=1504.6(5)3,Z=2,F(000)=950,S=1.011,最终偏离因子[I>2σ(I)]R1=0.0481,wR2=0.0952,对全部数据R1=0.0583,wR2=0.1000。     

配合物[Zn(p-ABA)2(phen)·(H2O)]·H2O的水热合成、晶体结构及热稳定性

在甲醇水混合溶剂中，以对乙酰氨基苯甲酸(p-ABA)，1，10-邻菲咯啉(phen)为配体与高氯酸锌合成了标题配合物[Zn(p-ABA)₂(phen)·(H₂O)]·H₂O。配合物(C₃₀H₂₆N₄O₈Zn，分子量为637.93)晶体属单斜晶系，空间群P2₁/c。晶体结构表明:锌原子与2个对乙酰氨基苯甲酸的2个氧原子，1个1，10-邻菲咯啉中的2个氮原子以及水分子中的氧原子配位，晶胞参数:a=1.362 77(17) nm， b=1.882 3(2) nm，c=1.252 53(16) nm;β=114.500(2)°，V=2.923 6(6) nm³，D_c=1.449 g·cm^-3，Z=4，F(000)=1 320，R₁=0.041 4，wR₂=0.087 8。形成五配位的三角双锥结构。对配合物热稳定性进行分析，结果表明，配合物在230.0 ℃以下稳定性好。     

双核镍配合物[Ni2(p-PhDTA)(2,2′-bipy)2(H2O)2]·4H2O的合成与晶体结构

A novel dinuclear complex of [Ni₂(p-PhDTA)(2,2′-bipy)₂(H₂O)₂]·4H₂O (p-PhDTA^2-=para-phenylenediamine-N,N,N′,N′-tetraacetate)has been synthesized. The complex was characterized by elemental analysis, IR spectra, thermo-analysis and X-ray diffraction. The crystal belongs to triclinic, space group P1 with a=0.976 3(7)nm, b=0.989 41(7) nm, c=1.084 29(8) nm, α=65.661 0(10)°, β=75.234 0(10)°, γ=85.616 0(10)°, Z=2, V=0.925 44(12) nm³, D_c=1.568 g·cm^-3, R₁=0.031 5, wR₂=0.081 4. In the complex, the central Ni(Ⅱ) ion is coordinated in a distorted octahedral geometry, defined by two carboxyl O atoms and one N atom from same p-PhDTA^2- group, two N atoms from 2,2′-bipyridine ligand and one water molecule. The two nickel (Ⅱ) ions are linked by p-PhDTA^2- group into a dinuclear structure and extensive hydrogen bonds link the complex into a 2D supramolecular network. CCDC: 294084.