含硫镍金属镍配合物[Ni(C13H7Br2NOS)2(DMF)]·(C3H7O)的合成与晶体结构

The complex, Ni[(C₁₃H₇Br₂NOS)₂(DMF)]·(C₃H₇O) (DMF=N,N′-dimethylformamide), was synthesized and characterized by the element analysis, IR and X-ray diffraction single crystal structure determination. The title complex crystallizes in monoclinic system, space group P2₁/n, with a=8.297 6(15) nm, b=12.866(2) nm, c=31.889(3) nm, β=95.024(2)°, and V=3 391.3(9) nm³, Z=4, R=0.075 2, wR=0.176 8. The nickel iron is six-coordinated by three O atoms, two N atoms, one S from the Schiff base and one O atom from DMF ligand, forming a octahedron coordination geometry. Schiff bases are bridged by the two S atoms. The molecules in the crystal are linked through intermolecular Br…Br, C-H…O, S…Br interactions. Its electrochemical property is reported. CCDC: 675768.     

一维链状酰基吡唑啉酮配合物Zn(C26H15N3O2Cl)2的合成、晶体结构及热稳定性

A one-dimensional chain complex bis{4-[(Z)-(4-chlorophenylamino)(2-furyl)methylene]-3-methyl-1-phenylpyrazol-5-onato}zinc(Ⅱ) Zn(C₂₆H₁₅N₃O₂Cl)₂ has been synthesized. Its structure was characterized by elemental analysis, IR, UV, thermal analysis and X-ray diffraction single crystal structure analysis. The title complex crystallizes in triclinic system, space group P1 with a=0.903 58(18) nm, b=1.359 8(3) nm, c=1.757 0(4) nm; α=102.42(3)°, β=101.24(3)°, γ=109.2(4)°, V=1.906 3(10) nm³. The final R factors are R=0.051 3 and wR=0.133 9. The zinc atom is four-coordinate involving two oxygen atoms and two nitrogen atoms forming a distorted tetrahedral geometry. The intermolecular hydrogen bonds C-H…N, C-H…Cl, C-H…π, together with intramolecular π…π stacking in the large congujate system, leading to the formation of a one-dimensional supramolecular chain. The results of TG-DTA analysis show that the title complex was stable under 323 ℃. CCDC: 299690.     

丙二酸根-1，10-邻菲罗啉合镍(Ⅱ)配合物的合成、晶体结构及光谱性质

A complex, NiL(Phen)₂(H₂O)₅ (Phen=1,10 phenanthroline; L=malonate), has been synthesized and chara-cterized. Single crystal X-ray structural determination has been carried out for the complex, the crystal is triclinic system, space group P1 with a=1.042 4(4) nm, b=1.061 2(4) nm, c=1.303 8(5) nm, α=85.784(4)°, β=77.232(3)°, γ=72.879(4)°, M_r=611.24, V=1.344 2(8) nm³, Z=2. In this complex, the central metal Ni(Ⅱ) atom is in distorted octa-hedron coordination environment. The molecule is extended to 2D network by the intermolecular π-π stacking interaction. CCDC: 278766.     

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.     

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.     

铜配合物[CuL2Cl2]·4H2O的合成和晶体结构(L=3-乙基-4-对甲氧苯基-5-(2-吡啶基)-1，2，4-三氮唑)

A new copper(Ⅱ) complex, [CuL₂Cl₂]·4H₂O, [L=3-ethyl-4-(p-methoxyphenyl)-5-(2-pyridyl)-1,2,4-triazole], was synthesized and characterized by X-ray crystallography and infrared spectroscopy. The complex crystallizes in triclinic system with space group P1, a=0.843 9(7) nm, b=0.965 5(8) nm, c=1.093 6(8) nm, α=84.026(19)°, β=82.33(2)°, γ=89.167(19)°, V=0.878 3(12) nm³, Z=1 with final R=0.033 8. The copper atom lies in a distorted octah-edral environment with two bidentate chelating ligands(L) in the equatorial plane and two Cl^- ions in the axial positions. The ligand L coordinates via one triazole nitrogen and one pyridine nitrogen atom. The molecules are stabilized by intermolecular hydrogen bonds in the crystal lattice. CCDC: 705817.     

5，6-二羧基苯并咪唑双核铕配合物的合成、结构及荧光性能

A europium complex [Eu₂(bmd)₂(Hbmd)₂(H₂O)₈]·8H₂O (H₂bmd=Benzimidazole-5,6-dicarboxylic acid) has been synthesized and structurally determined by X-ray diffraction single crystal structure analysis. The crystal belongs to triclinic, space grounp P1, with a=0.754 49(15) nm, b=1.253 8(3) nm, c=1.405 8(3) nm, α=71.03(3)°, β=82.83(3)°, γ=79.12(3)°, V=1.232 1(5) nm³, Z=1. The complex is a binuclear compound and each Eu(Ⅲ) ion is nine-coordinated. The versatile hydrogen bonds link binuclear units into a three-dimensional (3D) supermolecular network. Furthermore, the fluorescent properties of the complex have been investigated at room temperature. CCDC: 742510.     

3-甲基-4-对甲苯基-5-(2-吡啶基)-1，2，4-三唑-铜(Ⅱ)配合物

A copper(Ⅱ) complex [CuL(H₂O)(Sal)]·0.5H₂O was obtained by the reaction of copper(Ⅱ) salicylate with 3-methyl-4-(4-methylphenyl)-5-(2-pyridyl)-1,2,4-triazole (L) in ethanol-water solution at room temperature. The crystal belongs to triclinic system with space group P1, and a=0.913 6(4) nm, b=1.122 2(5) nm, c=1.263 3(7) nm, α=67.10(2)°, β=76.31(3)°, γ=68.17(2)°, V= 1.101(1) nm³, Z=2. The final refinement gave R₁=0.039 8 and wR₂=0.106 0 for 3 453 reflections with I>2σ(I). This complex is a good purple fluorescent material in solid state at room temperat-ure. CCDC: 685713.     

[Ni(C6H4N2)(CHC6H4O)2]配合物晶体结构及性质

The complex has been synthesized and characterized by spectroscopic techniques and single-crystal X-ray analysis. The crystal is orthorhombic ， space group P2₁2₁2₁ with a=1.6620(3)nm， b=1.7300(4)nm， c=0.5450(1)nm and Z=4. In the crystal lattice， the molecules create a two-dimensional network structure through hydrogen bonds. The C-H…O intermolecular hydrogen bonds connect the title complex to form layer super-molecular plane structure perpendicular to the axis b， with the layers stacked by the Van der Waals interaction. CCDC： 195309.     

配合物[Cu(CAM)(H2O)2]的水热合成与结构表征

A copper(II) complex [Cu(CAM)(H₂O)₂], (CAM=4-hydroxypyridine-2,6-dicarboxylic acid), has been hydr-othermally synthesized and characterized by elemental analysis, IR, and X-ray diffraction single crystal structure analysis. It belongs to triclinic system, with space group P1, a=0.783 3(3) nm, b=0.796 5(3) nm, c=0.798 6(3) nm, α=100.340(6)°, β=93.768(6)°, γ=109.348(5)°, V=0.458 3(3) nm³, Z=2. The copper(II) ion is 5-coordinated and exhi bits a distorted square pyramidal coordination environment. The two coordinated aqueous molecules and the oxygen atoms from the ligand generate the intermolecular hydrogen bonds, which result in the 2D supramolecular network. CCDC: 227156.     

一个双双核铜配合物的合成、结构及表征

Studies on the complexes containing formate have never been stopped for a half century. In this paper, a new copper(Ⅱ) complex, [Cu₂(phen)₂(HCOO)₂( μ-OH)₂][Cu₂(phen)₂(H₂O)₂(μ-OH)₂](HCOO)₂·10H₂O (1) (phen=1,10-phenanthroline), has been synthesized and characterized by elemental analysis, IR, and X-ray diffraction single crystal structure analysis. It belongs to triclinic system, with space group P1, a=1.151 7(3) nm, b=1.162 6(3) nm, c=1.216 0(3) nm, α=74.672(4)°, β=67.291(4)°, γ=79.029(4)°, V=1.441 4(6) nm³. The four copper(Ⅱ) ions in the complex are all 5-coordinated and exhibit a distorted square pyramidal coordination environment. The molecule are connected by intermolecular hydrogen bonds (C-H…O) interactions and π-π stacking, resulting in a three-dimensional network. CCDC: 648152.     

氢键构筑具有三维结构的配合物[Cu(N-phthgly)2(H2O)2]·C2H5OH的合成及晶体结构

A copper(Ⅱ) complex [Cu(N-phthgly)₂(H₂O)₂]·C₂H₅OH(N-Hphthgly=N-phthaloylglycine) has been synthesized and characterized by elemental analysis, infrared spectroscopy and X-ray crystallography. The complex crystallizes in triclinic space group P1 with a=0.472 90(7) nm, b=1.080 01(13) nm, c=1.154 02(15) nm, α=74.360 0(10)°, β=79.151 0(10)°, γ=87.918(2)°, V=0.557 37(13) nm³, Z=1. The central copper atom allows the formation coordination environment with two O(5) atoms of two water ligands and two O(1) atoms of two N-phthgly ligands. The complex forms a step-like 3D structure through the three types of O-H…O hydrogen bonds and the Cu…O weak interaction. CCDC: 712945.     

一个铜(Ⅱ)镍(Ⅱ)超分子化合物的合成、晶体结构与磁性

one new complex, [Cu(aeop)Ni(dpt)(H₂O)]·5H₂O, [H₄aeop=N′-(2-Aminoterephthalic acid)-N″-(1,3-Pro-panediamine) Oxamide], has been prepared by the diffusion method, where (aeop)^4- as bridging ligand, dpt as end ligand and characterized by elemental analysis, IR and X-ray crystal structure determination. It crystallizes in the Triclinic system, P1 space group with a=0.885 92(4)nm, b=1.232 53(6)nm, c=1.301 24(6)nm, α=85.593 0(10)°, β=78.753 0(10)°, γ=89.382 0(10)°, V=1.389 43(11) nm³, Z=2. The crystal structure analysis shows that intermolecular O-H…O and N-H…O hydrogen bonds result in a 3D supermolecular construction. The complex was characterized by magnetic susceptibility and presents a antiferromagnetic interaction (J=-46.4 cm^-1, g=2.24). CCDC: 727559.     

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.     

一维链状超分子化合物[Zn(dafo)2(H2O)2](NO3)2(dafo=4，5-二氮芴-9-酮)的合成、表征和晶体结构

A novel one-dimensional chain complex [Zn(dafo)₂(H₂O)₂](NO₃)₂ was synthesized. It has been characterized by IR, UV, TGA, Elemental analysis and X-ray diffraction analysis. The crystal belongs to triclinic system, P1 space group. The Crystallographic data are: a= 0.702 7(14) nm, b= 0.828 95(17) nm, c= 10.225(2) nm, α = 95.02(3)°, β = 91.45(3)°, γ = 99.85(3)°. The crystal structure data indicate that the Zn(Ⅱ) ion was coordinated with the four nitrogen atoms of two dafo and two oxygen atoms of two coordination water molecules, respectively. The complex has a one-dimensional chain structure, which is formed by hydrogen bonds.     

[Mn(H2O)(phen)2(PAc)](ClO4)的合成、红外光谱及晶体结构

The complex [Mn(H₂O)(phen)₂(PAc)](ClO₄) was synthesized and investigated by elemental analysis, molar conductivity, IR spectrum and X-ray diffraction methods, where phen=1,10-phenanthroline and PAc=phenylac-etate group. The complex crystallizes in the triclinic space group,P1 , with a=0.9289(2)nm,b=1.2425(2)nm,c=1.4791(3)nm,α=114.34(3)°,β=91.25(3)°,γ=104.65(1)°,V=1.4893(4)nm³,Z=2,F(000)=686,D_c=1.489g·cm^-3,μ=0.589mm^-1. The Mn(Ⅱ) ion has a six-coordinate distorted-octahedral geometry with the four nitrogen atoms of two phen ligands,a coordinated-water oxygen atom, and a carboxylate oxygen atom of PAc^-. There is π-π stacking interaction between two phen rings from two neighbor molecules.     

镧与β-丙氨酸配合物{[La2(β-ala)6(H2O)4](ClO4)6·H2O}n的合成及晶体结构

The complex, {[La₂(β-ala)₆(H₂O)₄](ClO₄)₆·H₂O}_n, was synthesized in aqueous solution and its crystal structure was determined by X-ray diffraction method .The crystal is triclinic with space group of .The cell pa-rameters are a=0.946(1)nm, b=1.2917(1)nm, c=2.1726(3)nm,α=76.79(1)°, β=80.85(1)°,γ=83.35(1)°, V=2.5429(5)nm³, Z=2, D_c=1.958g·cm^-3.The complex is an one-dimensional infinite chain. The coordination number of lanthanum ion is nine, forming a distorted tricapped trigonal prism.     

配合物[Cu2(phen)2](SiW12O40)(H2O)7的合成、晶体结构及电化学分析

The title complex has been synthesized by the reaction of silicotungstic acid, 1,10-phenanthroline (phen) monohydrate and cupric acetate. The crystal structure belongs to triclinic system, space group P1 with a=1.158 46(15) nm, b=1.658 8(2) nm, c=1.664 4(2) nm, α=82.090(2)°, β=76.001(2)°, γ=86.531(2)°, and V=3.072 6(7) nm³, D_c=3.887 g·cm^-3, Z=2, F(000)=3 196. R₁=0.086 7, wR₂=0.185 8. The structure shows that the copper(Ⅱ) atom is coordinated with two nitrogen atoms from the one phen and three oxgygen atoms from three water, forming a distorted square-pyramid configuration The cyclic voltametric behavior of the complex is also reported. CCDC: 298807.     

穴状Schiff碱配合物［Gd(NO3)·L］(NO3)2的晶体结构

A new mononuclear gadolinium complex ［Gd(NO₃)·L］(NO₃)₂ of Schiff base cryptand was obtained by condensation of tris (2-aminoethyl)amine with 2,6-diformyl phenol in template procedure. The complex was characterized by elemental analysis, IR, and x-ray single crystal diffraction analysis. Gadolinium is nine-coordinate in trigonal tricapped prism with five oxygen atoms from three phenols and a bidentate nitrate group, and four nitrogen atoms from three imino C=N bonds and a tertiary amine in the cryptand. The complex crystallized in triclinic system space group P1, a=1.0839(2) nm, b=1.2600(4) nm, c=1.7595(4) nm, α=82.09(2)°, β=89.22(2)°, γ=84.06(2)°， V=2.367(2) nm³, Z=2.     

配合物[Cu(HPHAc)2(py)2](H2PHAc=苯羟乙酸，py=吡啶)的合成和晶体结构

The novel copper(Ⅱ) complex with α-hydroxyphenylacetic acid (H₂PHAc) and pyridine (py) ligands, [Cu(HPHAc)₂(py)₂], has been synthesized and characterized by elemental analysis and IR spectroscopy. Its crystal structure was determined by single crystal X-ray diffraction techniques. The crystal belongs to monoclinic with space group C2/c. The cell parameters are: a=1.712 5(3) nm, b=1.533 2(2) nm, c=0.963 42(14) nm, β=111.866(2)°, V=2.347 6(6) nm³, and D_c=1.483 Mg·m^-3, Z=4, F(000)=1 084. The structure was refined to final R₁=0.071 4, wR₂=0.166 1. The complex has a six-coordinated distorted octahedral geometry, in which copper(Ⅱ) ion coordinates with two carboxylic oxygen atoms and two hydroxyl oxygen atoms from the two α-hydroxyphenylacetic acid ligands, two nitrogen atoms from the two pyridine ligands. The analysis of the crystal structure indicates that the complex has a one-dimensional chain structure, which is formed by intermolecular hydrogen bonds. CCDC: 255346.