新型配合物Mn2Hg4(SCN)12的合成与晶体结构分析

A new inorganic coordination compound Mn₂Hg₄(SCN)₁₂ was synthesized. The grown crystals were characterized by elemental analysis, infrared spectroscopic analysis and powder crystal X-ray diffraction in detail. The crystal structure of Mn₂Hg₄(SCN)₁₂ was determined by single-crystal X-ray diffraction. It belongs to monoclinic system, P2₁/c space group. The cell dimensions are: a=1.171 6 nm, b=1.431 05 nm, c=2.105 1 nm, β=100.738°, and Z=4. In the structure of it, half of Mn²⁺ cations have five-coordinate number, and other half of Mn²⁺ cations have six-coordinate number; 3/4 of Hg²⁺ cations are coordinated by four SCN^-, 1/4 of Hg²⁺ cations are coordinated by three SCN^- and one NCS^-, all the coordination geometry of Hg²⁺ show slightly distorted tetrahedrons. CCDC: 244939.     

含有双甜菜碱衍生物/SCN-混合配体的镉配合物的合成及晶体结构分析

A new coordination polymer of Cd(Ⅱ) was prepared by the reaction of Cd(ClO₄)₂·6H₂O with mixed ligands, namely, neutral double betaine derivative 1,3-bis(pyridinio-4-carboxylato)propane and SCN^- anion in aqueous solution. The crystal structure of 1 has been determined by single-crystal X-ray diffraction methods. Crystal data for 1: orthorhombic, space group P2₁2₁2₁, a=1.050 9(2), b=1.162 8(2), c=1.649 5(3) nm, V=2.015 7(7) nm³, Z=4, F(000)=1 064, D_c=1.756 g·cm^-3, the final R=0.050 8 and wR=0.130 1 for 3 530 observed reflections [I>2σ(I)]. Crystal structure of 1 indicates that the ( μ-1,3-NCS) bridging NCS^- ligand connects neighboring cadmium atoms, leading to a single strand helical chain which propagates along crystallographic a axis. The metallic nodes of adjacent helical chains are linked by monodentate-monodentate coordination mode of both carboxylate groups in L molecules to generate 2D coordination sheet which parallels to the (001) plane. Adjacent layers are further joined by C-H…O hydrogen bonds; the structure thus expanded into a three-dimensional network. CCDC: 612657.     

二维层状铜配位聚合物[Cu2(3-PyOH)2(EDTA)]n的合成与结构研究

A 2D copper coordination polymer of [Cu₂(3-PyOH)₂(EDTA)]_n (EDTA^4-=ethylenediaminetetraacetate quadrivalent anion C₁₀H₁₂N₂O₈, 3-PyOH=3-hydroxypyridine) was synthesized and characterized by the element analysis, IR and single crystal X-ray diffraction. The title complex crystallizes in monoclinic system with space group P2₁/c, a=1.327 5(3) nm, b=0.930 39(19) nm, c=0.948 44(19) nm, β=108.21(3)°, and V=1.112 8(4) nm³, Z=2, R=0.025 2, wR=0.066 1. Each copper(Ⅱ) atom is five-coordinated by three O atoms and one N atom from two different EDTA^4- groups and one N atom from 3-PyOH ligand, forming a distorted square-pyramidal coordination geometry. Two adjacent copper(Ⅱ) atoms are bridged by the bis-tetradentate EDTA^4- groups, constructing a two-dimensional layer structure along bc plane. The adjacent Cu…Cu distances are 0.502 5(3) and 0.611 3(3) nm. CCDC: 618806.     

一维链状2-氧-1(4H)-吡啶乙酸桥联钙配位聚合物[Ca(2-OPA)2(H2O)2]n的合成、晶体结构及热稳定性研究

A novel coordination polymer of [Ca(2-OPA)₂(H₂O)₂]_n (2-OPA-=2-oxo-1(4H)-pyridineacetate anion) was synthesized and characterized by elemental analysis, IR, TG and single crystal X-ray diffraction. The title complex crystallizes in orthorhombic with space group Pna2₁, a=0.799 96(16) nm, b=0.823 77(16) nm, c=2.415 3(5) nm, V=1.591 6(6) nm³, Z=4, R=0.030 3, wR=0.070 0. The Ca atom is eight-coordinated by six O atoms of four 2-OPA^- ligands and two water molecules, and displays a dodecahedron coordination geometry. Each 2-OPA^- ligand bridges two adjacent Ca atoms, forming a infinite chain along the a direction. The Ca…Ca distance is 0.4102 2(8)nm. A two-dimensional supramolecular framework is further constructed by the hydrogen bonds and the weak π-π interactions. The results of TG analysis show the chain structure of the title complex was stable under 297.5 ℃. CCDC: 251669.     

一维双链4-氧-1(4H)-吡啶氮乙酸桥联铜配位聚合物[Cu(4-OPA)2]n的合成、结构及性能研究

A novel coordination polymer of [Cu(4-OPA)₂]_n (4-OPA^-=4-oxo-1(4H)-pyridineacetate anion) was synthesized and characterized by elemental analysis, IR, TG, fluorescence and X-ray single crystal diffraction. The title complex crystallizes in triclinic with space group P1, a=0.713 17(14) nm, b=0.739 81(15) nm, c=0.753 02(15) nm, α=91.46(3)°, β=109.14(3)°, γ=111.31(3)°. V=0.344 92(17) nm³, Z=1, R=0.028 6, wR=0.080 3. The Cu atom occupies an inversion site in an octahedral environment, defined by two carbonyl O atoms and four carboxyl O atoms from different 4-OPA^- ligands. Adjacent Cu(Ⅱ) atoms are bridged by the 4-OPA^- ligands, forming a one-dimensional double chain structure. The closest Cu…Cu distance is 0.850 6(3) nm. The results of TG and fluorescent analysis show that the title coordination polymer is stable under 262.8 ℃ and has two emission peaks at 422 and 484 nm. CCDC: 287038.     

一维链状柔性羧酸镉配位聚合物[Cd(p-BDOA)·2H2O]n的合成、结构与性质研究(英)

A novel 1-D Cd(Ⅱ) coordination polymer, [Cd(p-BDOA)·2H₂O]_n(I) ( p-BDOA^2-=benzene-1,4-dioxyacetate dianion) has been synthesized and characterized by elemental analysis, IR, PL, TG and X-ray single crystal diffraction. The Crystal crystallizes in monoclinic system, the space group is C2/c, with the crystal cell parameters a=1.175 1(1) nm, b=0.551 0(1) nm, c=1.827 7(2) nm, β=96.14(2)°, and V=1.176 6(3) nm^3,, M_r=372.60, R=0.045 9, wR=0.127 9. The Cd(Ⅱ) ion has a trigonal prism coordination configuration that defined by four carboxyl O atoms from two different p-BDOA^2- ligands and two water molecules. Adjacent Cd(Ⅱ) ions are linked by carboxylate groups with the bidentate coordination mode, giving rise to a chain structure with the adjacent Cd…Cd distance of 1.526 3(5) nm. Furthermore, such chains are linked by hydrogen bonds to form supramolecular network. The results of PL and TG show that the complex exhibits intense fluorescent emissions and its chain skeleton is thermally stable up to 419 K. CCDC: 220443.     

一维链状锰配位聚合物[Mn(4-CPOA)(2，2-bipy)(H2O)]n的合成与晶体结构(英)

A novel 1D coordination polymer of [Mn(4-CPOA)(2,2-bipy)(H₂O)]_n (4-CPOA^2-=4-carboxylphenoxyacetate) has been synthesized and characterized by elemental analysis, IR and single crystal X-ray diffraction. The crystal crystallizes in monoclinic system, the space group is C2/c, with the crystal cell parameters a=1.437 9(2) nm, b=1.323 4(2) nm, c=1.970 5(3) nm, β=104.00(3)° and V=3.638 3(10) nm³, M_r=423.28, R=0.065 9, wR=0.130 3. The Mn(Ⅱ) ion displays a distorted octahedral coordination configuration, defined by three carboxyl O atoms from different 4-CPOA^2- groups, two N atoms from the 2,2-bipyridine ligand and one water molecule. Adjacent Mn(Ⅱ) ions are linked by carboxylate groups into a chain structure with the Mn…Mn separation of 0.977 1(3) nm. The two-dimensional supramolecular network is constructed through intermolecular hydrogen bonds and π-π stacking interactions. CCDC: 224464.     

镧系四元混合阴离子配合物［Ce(p-MBA)2(NO3)(phen)］2的合成和晶体结构

We synthesized new mixed anion complex of lanthanide ［Ce(p-MBA)₂(NO₃)(phen)］₂ in slightly acidic solution of ethanol and determined the single crystal structure. The title complex is triclinic, space group P1, a=1.1027(4) nm, b=1.2511(5) nm, c=1.0633(3) nm, α=106.90(3)°, β=96.73(3)°, γ=86.85(3)°, V=1.3937(9) nm³, D_C=1.555 g·cm^-3, Z=1, F(000)=650.00 and μ(MoKα)=16.82 cm^-1. The four p-MBA ligands have two kinds of coordination modes and the coordination number of the Ce³⁺ is nine. There is some aromatic-stacking interaction in the benzene rings of two p-MBA ligands.     

二维网状铜(Ⅱ)配位聚合物{Cu(μ2-C10H8N2O3)( μ2-C6H12N4)1/2}n的合成和晶体结构

The novel copper(Ⅱ) coordination polymer with 2-oxo-propionic acid benzoyl hydrazone and hexamethylenetetramine ligands, {Cu(μ₂-C₁₀H₈N₂O₃)( μ₂-C₆H₁₂N₄)_1/2}_n (C₁₀H₈N₂O₃^2- is the dinegative ion of 2-oxo-propionicacid benzoyl hydrazone), has been synthesized and characterized by elemental analysis and IR spectroscopy. The crystal structure was determined by single crystal X-ray diffraction analysis. The results show that the crystal of the title coordination polymer belongs to monoclinic space group C2/c, the cell parameters are as follows: a=1.787 5(2) nm, b=0.730 93(9) nm, c=2.038 2(2) nm, β=92.890(2)°, and V=2.659 6(5) nm³, Z=8, D_c=1.687 Mg·m^-3, μ(Mo Kα)=1.659 mm^-1, F(000)=1 384, R=0.031 1, wR=0.079 0 for 2 454 observed reflections (I>2σ(I)) out of 2887 unique reflections. In this copper(Ⅱ) coordination polymer, each copper(Ⅱ) ion is five-coordinated with a geometry of distorted square-pyramid. Two oxygen atoms of the carboxyl of each C₁₀H₈N₂O₃^2- acts as a bridge to bond two neighboring copper(Ⅱ) ions, leading to an infinite one-dimensional chainlike coordination polymer. Each chain is linked by coordinated hexamethylenetetramines with its neighbors to form an infinite two-dimensional network structure. CCDC: 255347.     

配位聚合物{[Zn(CF3COO)2(C5H5ON)]·H2O}n的合成、晶体结构及表征

new coordination polymer {[Zn(CF₃COO)₂(C₅H₅ON)]·H₂O}_n was synthesized based on the reaction of zinc(Ⅱ) trifluoroacetate and 3-hydroxypyridine(C₅H₅ON) in methanol medium for the first time. The structure of the coordination polymer was confirmed by IR, ¹H NMR, elemental analysis and thermal analysis. The crystal structure of the coordination polymer was also determined by X-ray single crystal diffraction. The crystal belongs to monoclinic system with space group P2₁/m, and crystallographic data of the coordination polymer are: a= 0.863 1(4) nm, b=0.717 7(3) nm, c=1.116 4(5) nm, α=γ=90°, β=107.542(6)°, V=0.659 4(5) nm³; D_c=2.037 g·cm^-3; Z=2; F(000)=400; μ=1.969 mm^-1. Zinc(Ⅱ) atom lies at the center of an octahedron formed by the coordination of zinc atom and six O atoms which come from four different trifluoroacetate ions and two different 3-hydroxypyridine molecules where each trifluoroacetate ion and 3-hydroxypyridine are coordinated to two different zinc ions to form coordination polymer. CCDC: 253909.     

[Cu(Ⅱ)(DETA)]3[Cr(CN)6]2·5H2O(DETA=二乙烯三胺)氰桥配合物的结构和磁性研究

A new coordination complex [Cu(Ⅱ)(DETA)]₃[Cr(CN)₆]₂·5H₂O (DETA=diethylenetriamine) was synthesized, its crystal structure and magnetic properties were determined. The crystal crystallizes in monoclinic space group P2₁/c, with unit cell constants a=2.056 6(7) nm, b=1.440 7(5) nm, c=1.513 3(5) nm, β=95.996(6)°, and V=4.459(3) nm³, Z=4, D_c=1.499 g·cm^-3, F(000)=2 060，μ(Mo Kα)=1.936 mm^-1, R₁=0.052 3, wR₂=0.106 2. The structure consists of a one-dimensional chain of [Cu(DETA)]₂[Cr(CN)₆]⁺ and binuclear [Cu(DETA)][Cr(CN)₆]^-. The coordination geometries around Cu²⁺ atoms are distorted square-based pyramidal and distorted square, respectively. Magnetism studies show that there are ferromagnetic interactions between Cu²⁺ and Cr³⁺ ions. CCDC: 272213.     

DBBD及其Cu(I)配位聚合物[CuI(DBBD)2]n的合成

In this article we report the synthesis of (R,S)-4,4′-biquinoline-6,6′-dimethyl-3,3′-dicarboxylate (DBBD) (1) and the formation of copper(I) coordination polymer [CuI(DBBD)₂]_n (2) by inducing a bidentate organic ligand (DBBD). The crystal 1 belongs to monoclinic system with space group P2₁, and a=0.881 30(19) nm, b=1.966 0(6) nm, c=1.478 1(4) nm, β=119.429(12)°, V=2.230 5(10) nm³, D_c=1.276 g·cm^-3. The crystal 2 belongs to orthogonal system with space group Fmm2, and a=2.044 41(17) nm, b=1.543 06(13) nm, c=1.652 45(13) nm, V=5.212 9(7) nm³, D_c=1.669 g·cm^-3, Z=8. CCDC: 292931, 1; 292934, 2.     

[Mn(NH2NHCO2C2H5)3](NO3)2的晶体结构和热分解机理

[Mn(ECZ)₃](NO₃)₂ is newly prepared by the aqueous solutions of Mn(NO₃)₂ and ethyl carbazate (ECZ). The crystal structure has been determined by X-ray crystal diffraction analysis. It belongs to monoclinic with space group of P2₁/n. The crystal parameters are: a=1.3974(2) nm, b=0.8796(2) nm, c=3.4322(7) nm, β=91.25(1) °, V= 4.2175(1) nm³, Z=8. Its molecular weight is 491.30. Mn²⁺ is located on the center of the molecular structure. Ethyl carbazate serves as a bidentate ligand which coordinates to the metal cations with its carbonyl oxygen atom and the terminal hydrazine nitrogen atom, forming five-member chelating rings, and three such rings are formed in each molecule. The coordination number of the metal ion is six and the coordination configuration of the central ion is octahedral. Specially, antimer configuration phenomenon is found in the molecule. The complex is further characterized by element analysis and IR measurements. The thermal decomposition mechanism is studied by using TG-DTG and DSC techniques. CCDC: 215675.     

草酸根桥联的双核铜(Ⅱ)配合物[Cu2(phen)2(H2O)2(μ2-C2O4)](NO3)2的合成及晶体结构

A new binuclear copper(Ⅱ) complex, [Cu₂(phen)₂(H₂O)₂(μ₂-C₂O₄)](NO₃)₂, has been synthesized and characterized by elemental analysis, IR and UV-Vis spectrum. Its crystal structure was determined by single crystal X-ray diffraction techniques. Crystal data: monoclinic, space group P2₁/c, a=0.712 21(8) nm, b=1.170 93(14) nm, c=1.783 7(2) nm, β=111.828(2)°, and V=1.380 8(3) nm³, D_c=1.769 Mg·m^-3, Z=2, F(000)=744, R₁=0.025 4, wR₂=0.069 5, Gof=1.077, Δρ=328～-455 e·nm^-3. The complex is packed by one centrosymmetry binuclear copper(Ⅱ) unit, oxalate dianion and NO₃^- anion. In the molecule structure of the title complex, two Cu(Ⅱ) ions are bridged by oxalate dianion and each Cu(Ⅱ) ions coordinates with two nitrogen atoms from 1,10-phenanthroline ligand and one oxygen atom from water to form a five-coordinate distorted square-pyramidal configuration. The hydrogen bonds are observed between coordinated water molecules and NO₃^- anions. The analysis of the crystal structure indicates that the complex has a two-dimensional stacking network structure, which is formed by intramolecular hydrogen bonds, intermolecular hydrogen bonds and stacking effect of aromatic ring. CCDC: 255345.     

高氯酸稀土Sm(Ⅲ)开环冠醚(EO4)配合物的晶体结构

The crystal of title compounds belongs to orthorhombic system with space group P2₁2₁2₁ (No.19). The cell parmeters are a=1.432 16(3) nm, b=1.457 20(3) nm， c=3.005 85(6) nm, and V=6 273.0(2) nm³, Z=8, μ(Mo Kα)=22.21 cm^-1， D_c=1.802 g·cm^-3, F(000)=3 416.00, Finally R₁=0.033 and wR₂=0.073 (I>2.00σ(I)), S=1.023. Every center atom Sm(Ⅲ) is surrounded by the two aether chains, the title compound has ten-coordinate structure and the coordination polyhedron shows a Bicapped Square Antiprism. In the crystal, the title compound has the flack of double moleculars and non-symmetry. The anion ClO₄^- does not take part in the coordination. CCDC: 238709.     

钾的N-酰化牛磺酸配合物的合成、表征及其晶体结构

The title complex(K(C₉H₁₃NO₅S₂)(H2O)) was synthesized by the reaction of p-tolysulfonyl chloride, taurine and potassium hydrate in water-methanol-ethanol solution. The crystal structure was determined by X-ray diffraction method and the chemical formula weight of the complex is 336.44. The crystal structure of the title complex belongs to orthorhombic space group Pbca and cell parameters: a=0.853 31(12) nm, b=0.820 42(12) nm, c=3.989 4(6) nm. V=2.792 8(7) nm³, Z=8, D_c=1.600 g·cm^-3, μ=0.699 mm^-1, F(000)=1 400. The compound is an one-dimension chain complex of infinite length which are connected with hydrogen bond and bridging coordination water. The difference and same of the complexes were discussed. CCDC: 244938.     

九配位钬-三乙四胺六乙酸配合物K3[Ho(TTHA)]·5H2O的合成及分子结构

In this paper, the molecular and crystal structures of the K₃[Ho(TTHA)]·5H₂O(TTHA=triethylenete-traminehexaacetic acid)are given. The crystal data are as follows: monoclinic system, P2₁/c space group, a=1.0290(9)nm, b=1.2466(11)nm, c=2.279(2)nm, β=91.322(16)°, V=2.923(5)nm³, Z=4, M=860.67, D_c=1.956gcm^-3, μ=3.217mm^-1, F(000)=1720. The final R₁ and wR₂ are 0.0395 and 0.0796 for 5145 [I >2.0σ(I)] unique reflections and 0.0546 and 0.0833 for all 11567 reflections, respectively. In the title complex, the anion [Ho(TTHA)]^3- has a nine-coordination structure with distorted tricapped trigonal prism. A TTHA having four N atoms of amido groups and six O atoms of carboxylic groups acts as a enneadentate ligand with four N atoms and five O atoms. In addition, there is a free non-coordinated carboxyl group (-CH₂COO^-) in the complex anion [Ho(TTHA)]^3-. The free carboxyl group could be embellished by some biological molecules which have selectivity and affinity to tumor cell. Then the ¹⁶⁶Ho^Ⅲ- TTHA complex may become radioactive anti-tumor drug having targeting function.     

配位聚合物[NaMn(pic)3]n的水热合成和晶体结构

A Coordination polymer [NaMn(pic)₃]_n (1) (picH=picolinic acid) has been synthesized by hydrothermal synthesis and structurally characterized by single crystal structure determination. 1 crystallizes in the orthorhombic space group Pbca, a=1.251 9(4) nm, b=1.715 8(8) nm, c=1.754 7(7) nm, V=3.769(6) nm³, M_r=444.24, D_c=1.566, F(000)=1 800, R₁=0.024 8 and wR₂=0.075 1 for I>2σ(I). According to the crystal structure, each Mn(Ⅱ) ion of 1 is six-coordinated with three oxygen and three nitrogen atoms from three pic anions to form a distorted dodecahedron. Each Na⁺ ion of 1 is penta-coordinated with two oxygen atoms from a pic anion and three oxygen atoms from three pic anions of diffrent unit to form a distorted tetragnal pyramid. The three-dimensional coordination polymer 1 is connected through Na⁺ ion. CCDC: 683029.     

配合物[1-(4′-fluorobenzyl)pyridinium]2[Ni(dto)2](dto2-=dithiooxalate dianion)的合成及晶体结构

The complex [1-(4′-fluorobenzyl)pyridinium]₂[Ni(dto)₂] (dto^2- means dithiooxalate dianion) has been pre-pared by reaction of Na₂[Ni(S₂C₂O₂)₂] and the 1-(4′-fluorobenzyl)pyridinium chloride salt. The crystallographic data for the title complex: triclinic P1, a=8.5698(8)?, b=9.3461(9)?, c=10.5361(10)?, α=67.177(2)°, β=67.398(2)°, γ=79.611(2)°, V=717.59(12)?³, Z=1. The [Ni(dto)₂]^2- anion with the Ni atom lying on an inversion center and exhibits a quasi-planar structure. An extensive hydrogen bond network of C-H…O is clearly observed. The nature and size of cation seems to play an important factor in the type of intermolecular interactions as well as the crystal packing in this kind of complexes.     

[Cu(TO)2(H2O)4](PA)2的合成和晶体结构

[Cu(TO)₂(H₂O)₄](PA)₂ was prepared by mixing the aqueous solution of 1,2,4-triazol-5-one(TO) and Cu(PA)₂. The molecular structure and crystal structure of the title complex was determined by X-ray single crystal diffraction method. The crystal is triclinic, space group with a=0.7321(1)nm,b=0.7474(2)nm,c=1.3649(3)nm;α=88.65(2)°,β=85.63(1)°,γ=63.35(1)°;V=0.6655(2)nm³,Z=1. The Cu²⁺ coordinated with two TO molecule through its 2-nitrogen atom and four water molecules and showed an octahedral configuration.