新颖一维配位聚合物[Ni(3，5-pdc)(H2O)4]·(H2O)的合成与晶体结构

The hydrothermal reaction of 3,5-pyridinedicarboxylic acid and NiCl₂·6H₂O results in a novel coordination polymer， [Ni(3,5-pdc)(H₂O)₄]·(H₂O). The crystal structure of the compound was determined by X-ray single crystal diffraction. The crystal belongs to monoclinic system with space group P2₁/n, a=1.136 1(3)nm, b=0.709 8(2) nm, c=1.459 7(4) nm, β=107.538(4)°， V=1.122 4(6) nm³, D_c=1.858 g·cm^-1, Z=4, F(000)=648, R₁=0.0264, wR₂=0.0665. CCDC: 224880.     

一维链状配位聚合物[Cu3(TFSSB)2·(H2O)4·4H2O]n的合成和晶体结构

The title complex [Cu₃(TFSSB)₂·(H₂O)₄·4H₂O]_n (TFSSB=taurine 3-formylsalicylic schiff base) was synthesized by TFSSB and copper(Ⅱ) acetate monohydrate in ethanol solution and the crystal structure was determined by X-ray diffraction method. The crystal belongs to monoclinic system, space group P2₁ / n，with cell parameters: a=0.927 9(6) nm, b=1.173 0(2) nm, c=1.471(2) nm, β=106.96(2)°, and V=1.531(2) nm³, Z=2, D_c=1.890 g·cm^-3, μ=2.291 mm^-1, F(000)=882, R₁=0.025 9, wR₂=0.065 9. The Cu1 is five-coordinate, the Cu2 is four-coordinate. CCDC: 253298.     

一维链状镉(Ⅱ)配位聚合物[Cd(μ-DPIA)2(H2O)]n的合成与结构研究

A novel one-dimensional coordination polymer, [Cd( μ-DPIA)₂(H₂O)]_n (HDPIA=4,5-Diphenylimidazole-1-acetic acid), was synthesized and characterized by the element analysis, IR and single crystal X-ray diffraction. It crystallizes in the orthogonal space group Pca2₂ with unit cell parameters: a=1.509 6(3) nm, b=0.611 1(1) nm, c=3.216 4(6) nm, and V=2.967 1(10) nm³, Z=4, R=0.032 7, wR=0.086 7. The Cd atom is seven-coordinated by four O atoms and two N atoms from two chelating DPIA^- ligands and one water molecule, and displays a distorted pentagonal bipyramid coordination geometry. Each DPIA^- ligand bridges two adjacent Cd atoms, forming a infinite chain along the a axis direction. The Cd…Cd separation within the polymer is 0.765 0(3) nm. A layer structure which parallels to the ab plane is further constructed by hydrogen bonding interactions. CCDC: 254247.     

一维交替链状稀土配位聚合物[Er(dpa)(pya)(H2O)]n和[Nd2(pya)6(H2O)4]n的水热合成及结构表征

在水热条件下，稀土氧化物与2，2′-联苯二甲酸及异烟酸反应得到了两个新颖的一维交替链状配位聚合物[Er(dpa)(pya)(H₂O)]_n和[Nd₂(pya)₆(H₂O)₄]_n(H₂dpa=2，2′-联苯二甲酸；Hpya=异烟酸)。测定了它们的晶体结构，并进行了红外光谱和元素分析等 性质的表征。晶体结构测定表明这两个化合物同属单斜晶系，并具有相同的空间群P2₁/n， 晶体学参数分别为配合物1：a= 0.8830(3) nm，b=1.058 5(3) nm，c=2.089 1(6) nm，β=98.429(4)°，D_c=1.883g·cm^-3， V=1.931 4(10) nm³，Z=4； 配合物2：a=0.968 9(4) nm，b=1.978 3(9) nm，c=1.164 2(6) nm，β=112.106(7)°，D_c=1.756 g·cm^-3，V=2.067 5(17) nm³，Z=4。     

配位聚合物[Mn(4，4′-bpy)1.5(H2O)3](ClO4)·(4，4′-bpy)(L)·H2O的水热合成和晶体结构

The title compound, [Mn(4,4′-bpy)_1.5(H₂O)₃](ClO₄)·(4,4′-bpy)(L)·H₂O(1), where L=2,4,6-trimethylbenzoic acid, was synthesized and its crystal structure was determined by X-ray diffraction analysis. The crystal is of triclinic, space group P1 with a=2.929 9(6) nm, b=1.036 4(2) nm, c=8.222 0(1) nm, α=105.300(2)°, β=97.495(2)°, γ=91.118(2)°, V=1.884 0(4) nm³, Z=2, M_r=780.10, D_c=1.375 g·cm^-3, μ=0.483 mm^-1, F(000)=812, R=0.055 4, wR=0.135 2. The Mn atoms are octahedrally coordinated by three N atoms of three 4,4′-bipyridine ligands and three O atoms of water. The complex shows a one-dimensional chain structure bridged by water and 4,4′-bipyridine molecules. CCDC: 615707.     

一种新颖1D链状聚合物[Ni(acac)2(dadpm)]∞的合成与晶体结构

The title compound [Ni(acac)₂(dadpm)]_∞ (acac=acetylacetonate, dadpm=4,4′-diaminodiphenylmethane) was synthesized from Ni(acac)₂·2H₂O with dadpm in DMF. The structure was characterized by elemental analysis, IR spectroscopy, thermal analysis and single-crystal X-ray diffraction. X-ray analysis revealed that the central Ni atom is at a center of symmetry, and is octahedrally coordinated by four O atoms from two acac anions and two N atoms from two dadpm ligands. Each dadpm ligand, which has a two-fold axis passing through its methylene C atom, bridges two Ni atoms to form a 1D polymeric chain. Neighboring chains connect via H bonding interactions to generate a 2D network. It crystallizes in the monoclinic system, space group P2/c with a=0.556 79(7), b=0.896 06(12), c=2.187 3(3) nm, β=94.942(3)°, V=1.087 2(3) nm³, Z=2, D_c=1.390 g·cm^-3, F(000)=480, M_r=455.17, μ(Mo Kα)=0.924 mm^-1, R(F)=0.036 0, wR(F²)=0.101 0, S=1.013. CCDC: 254565.     

配位聚合物[Mn(2，4，6-TMBA)2(H2O)3]n·2nH2O的水热合成和晶体结构

The title compound, [Mn(2,4,6-TMBA)₂(H₂O)₃]_n·2nH₂O(1), where 2,4,6-TMBA=2,4,6-trimethylbenzoic acid, was synthesized and its crystal structure was determined by X-ray diffraction analysis. The crystal is of monoclinic, space group C2/c with a=2.929 9(6) nm, b=1.036 4(2) nm, c=8.222 04(17) nm, V=2.494 7(9) nm³, Z=4, M=471.40, D_c=1.255 g·cm^-3, μ=0.571 mm^-1, F(000)=996, R_int=0.029 4, R=0.037 6 and wR=0.094 9. The Mn atoms are octahedrally coordinated by two O atoms of two ligands and four O atoms of water. The carboxyl group coordinates to Mn(Ⅱ) in the mode of monodentate, while the O atoms of water molecules coordinates in bridging mode. The complex shows a one-dimensional chain structure bridged by water molecules. CCDC: 297750.     

一种新的有机-无机混配配位聚合物[Zn(N3)2(bpp)]n的自组装及晶体结构(bpp=1，3-二吡啶丙烷)

A novel coordination polymer [Zn(N₃)₂(bpp)]_n[bpp=1，3-bis(4-pyridyl)-propane] was synthesized at room temperature and structurally characterized by means of X-ray single crystal diffraction. The results show that the polymer exhibits a linear chain structure; the Zn-Zn distance is 12.235?. Each Zn(Ⅱ) ion is coordinated by two nitrogen atoms from bpp ligands and two nitrogen atoms from azido (N₃^-) groups， the coordination geometry of Zn(Ⅱ) ion is a slightly distorted tetrahedron， the angles around Zn(Ⅱ) ions are from 103.27° to 121.37°. In the solid-state structure of the polymer， the linear chains are stacked with parallel mode along a direction. Moreover， between adjacent chains， there are π-π interactions between pyridine rings， which are arranged in face-to-face fashion with interplanar distances of av. 3.821?. CCDC： 189591.     

三维化合物[Ni2(BDC)2(m-bix)(H2O)3·3H2O]n的合成、结构和性质

水热条件下,合成了一个三维配位聚合物[Ni₂(BDC)₂(m-bix)(H₂O)₃·3H₂O]_n(1)[BDC=对苯二甲酸,m-bix=1,3-双(咪唑基-1-甲基)-苯],并通过红外,热重和X-射线单晶衍射进行了表征。X射线衍射结果表明化合物含有类似配位环境的金属2个Ni²⁺离子,2个BDC^2-配体,1个m-bix分子,3个配位水分子和3个游离的溶剂水分子。两个Ni²⁺离子分别采用八面体构型,通过桥联水分子形成双核单元,然后通过全部脱质子的BDC形成三维孔洞结构,m-bix配体通过连接两类双核金属原子形成三维框架,游离水分子存在于框架之中。有趣的是,化合物的结构是单一六节点,具有自穿插特征。而且对化合物的红外和热重性质进行了表征。     

原位产生的SO42-配位的二维无机钴配合物K2[Co3(OH)2(SO4)3(H2O)2]的水热合成及晶体结构

相同的水热反应条件下4-氨基-二(2-吡啶基)-1，2，4-三氮唑(abpt)、KSCN与钴盐(CoCl₂·6H₂O)反应合成了2种新的钴配合物:零维的单核配合物[CoSCN(abpt)] (1α)和二维的无机层状配合物K₂[Co₃(OH)₂(SO₄)₃(H₂O)₂] (1β)，并通过元素分析和红外光谱对其进行了表征。配合物1α的晶体属于单斜晶系，P2₁/c空间群。配合物1β晶体属于正交晶系，Cmc2₁空间群。在配合物1α中，abpt和SCN^-配体都参与配位与Co(Ⅱ)离子形成了2个不同的单核单元，这些单核单元又通过S原子和N原子之间的氢键作用连成了三维超分子结构;在配合物1β中，abpt配体没有参与配位，而SCN^-配体则被氧化成了SO₄^2-离子并与Co(Ⅱ)离子配位形成了二维配位层状结构，相邻层之间进一步通过氢键作用形成了沿c轴方向有孔道的三维超分子网络，这些孔道里面填充着反离子K+。     

配合物[Mn(phendione)(PDC)(H2O)2]·2H2O的合成与晶体结构

The title compound [Mn(phendione)(PDC)(H₂O)₂]·2H₂O (H₂PDC=pyridine-2，6-dicarboxylic acid) has been prepared in aqueous solution and characterized by single X-ray diffraction structure determination， elemental analysis， IR spectroscopy， and thermal analyses. The compound crystallizes in Monoclinic system， space group C2/c， a=1.017 51(11) nm， b=1.483 25(11) nm， c=1.461 21(13) nm， β=109.86(10)°， V=2.074 1(3) nm³， Z=4， F(000)=1 028， μ=0.701 mm^-1， D_c=1.609 g·cm^-3， R₁=0.028 9， wR₂=0.078 8 [I>2σ(I)]. Crystal structure reveals that complex consists of one-dimensional chain framework bridged by hydrogen bonds that formed by uncoordinated water and oxygen atom of carboxyl group in PDC^2-. Furthermore， the complexes form a three-dimensional super-molecular structure through hydrogen bonds. CCDC: 648570.     

配合物Fe(pda)2(H2O)4和[FeCo(pda)4(H2O)4]n的合成与晶体结构

采用水热法合成了2个3-(3-吡啶基)丙烯酸的配合物:Fe(pda)2(H2O)4(1)和[FeCo(pda)4(H2O)4]n(2)(pda=3-(3-吡啶基)丙烯酸),用红外光谱、元素分析、热重-差热以及X-射线衍射单晶结构分析进行了表征.2个配合物都属于单斜晶系,配合物1的空间群为P21/n,配合物2的为P21/c.配合物1是一个pda配体中仅吡啶基氮原子参与配位、而羧基上的氧原子未参与配位的单核结构,通过大量的氢键作用形成三维超分子体系.2是pda配体桥联Fe和Co的异核二维层状配位聚合物;配体吡啶基上的氮原子和羧基上的氧原子都参与了配位,其中羧基采用单齿配位模式.     

一维链状配位聚合物[M(H2bpb)(H2O)4](SO4)2·6H2O[M=Zn(Ⅱ)，Cu(Ⅱ)]的合成及晶体结构表征

设计并合成了一个含吡啶基团的柔性配体：N，N′-Bis(3-pyridylmethyl)-1，4-benzenedimethylamine(bpb)。通过bpb与硫酸锌及硫酸铜反应得到了两个新型具有一维链状结构的配位聚合物：[M(H₂bpb)(H₂O)₄](SO₄)₂·6H₂O[M=Zn(Ⅱ) 1，Cu(Ⅱ) 2]。X-射线晶体结构测定表明，这两个     

新型二维杂金属配位聚合物[La(Hida)Co(ida)2]·0.5H2O的水热合成与表征

采用水热法合成出一种新型二维杂金属配位聚合物[La(Hida)Co(ida)2].0.5H2O(ida=氨基二乙酸),并通过X射线单晶结构分析、红外光谱分析、元素分析、热重分析以及X射线粉末衍射分析对该化合物进行了表征.结构分析数据表明,该化合物属单斜晶系,C2/c空间群,晶胞参数a=0.97078(19)nm,b=2.4128(5)nm,c=0.85964(17)nm,β=114.91(3),°V=1.8263(6)nm3,Z=4,R=0.0126.该化合物是由一维La-Co杂金属链通过四齿羧酸配体连接形成的新型二维杂金属配位聚合物.     

稀土配位聚合物[M(tddc)(NO3)(H2O)4]·2H2O(M=Eu，Dy)的合成、结构和性质

本文用水热法合成了2个稀土配位聚合物[M(tddc)(NO₃)(H₂O)₄]·2H₂O[M=Eu (1),M=Dy (2)],并对它们进行了元素分析、红外光谱、热重等分析,研究了它们的荧光性质,并用X-射线单晶衍射测定了配合物的单晶结构。两者的晶系都属于三斜晶系,P1空间群。荧光实验表明配合物1在常温下具有很强的荧光。     

咪唑-4，5-二羧酸锰的2D配位聚合物[Mn(HIDC)(H2O)]n的合成与晶体结构

由含氮杂环的有机羧酸分子建筑块与金属离子构筑的配位聚合物不仅具有多样的拓扑结构类型,而且在光学、磁学、吸附分离、催化等领域中显示出潜在的应用价值[1,2]。咪唑-4,5-二羧酸(H3IDC)具有N/O两种配位原子和广泛的生物学特性,且随着酸度的变化以不同的酸根离子存在(H2IDC-,HIDC2-,IDC3-),从而形成多样的配位模式,可以作为一种较好的有机羧酸桥配体与金属离子构筑配位聚合物。迄今为止,已有咪唑-4,5-二羧酸与钴、钠构筑的四方型配合物[3],与镉的单核和一维配合物[4,5],与锰形成的单核[6,7]、双核[8,9]、一维链状[10]配合物结构的报…     

一维链状铜配位聚合物[Cu(m-BDOA)(bipy)·H2O]n的合成与晶体结构

A novel coordination polymer, [Cu(m-BDOA)(bipy)·H₂O]_n (m-BDOA^2-=benzene-1,3-dioxyacetate), was synthesized and characterized by elemental analysis, IR spectra, X-ray single crystal structure analysis. Crystallographic data are as follows: orthorhombic, space group Pna2₁, a=1.606 9(3) nm, b=1.685 9(3) nm, c=0.699 7(1) nm, V=1.8955(7) nm³, Z=4, D_c=1.619 g·cm^-3, μ=1.200 mm^-1, F(000)=948，R=0.038 1, wR=0.038 6. The copper atom is five-coordinated involving two oxygen atoms of different m-BDOA^2- ligand, two nitrogen atoms of 2,2′-bipy ligand and one coordinated water, there is a distorted square pyramidal environment. Two copper atoms are bridged by m-BDOA^2- ligand, forming a one-dimensional chain along a axis. The adjacent distance of Cu…Cu atoms is 0.877 3nm. The crystal network was formed by the intermolecular hydrogen bond and π-packing interactions.     

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.     

氢键构筑的新颖微孔配位聚合物[Co2(Hisor)2·(4,4′-bpy)2(H2O)2]·4,4′-bpy的合成与结构

A novel microporous coordination polymer [Co2(Hisor)2(4,4′-bpy)2(H2O)2]·4,4′-bpy was synthesized by hydrothermal reaction and characterized by single crystal X-ray diffraction, elemental analysis and IR spectrum. The crystal belongs to the monoclinic system and space group is P2/n with a=1.040 6(3) nm, b=1.138 8(4) nm, c=1.854 7(6) nm, β=102.991(6)°, V= 2.141 6(12) nm3, Z=2, Dc=1.443 Mg/m3, Mr=930.62, μ=0.842 mm-1, F(000)=952, GOF= 1.072, R=0.065 4, wR=0.146 8[I>2σ(I)]. There are two crystallographically independent Co(Ⅱ) ions in the title complex. The Hisor2- and 4,4′-bpy link the metal ions into 2D grids with dimension of 0.522 3 nm×1.138 8 nm. There are O—H…O and N—H…O hydrogen bonds in the complex resulting in the formation of 3D network with 1D channels, in which are free 4,4′-bpy molecules.