三元混合配合物Cu(C10H8N2O3)·(C5H5N)·(H2O)的合成和晶体结构

The novel copper(Ⅱ) complex with 2-oxo-propionic acid benzoyl hydrazone and pyridine ligands, Cu(C₁₀H₈N₂O₃)·(C₅H₅N)·(H₂O) (C₁₀H₈N₂O₃^2- is the dinegative ion of 2-oxo-propionicacid benzoyl hydrazone), has been synthesized and characterized by elemental analysis and IR. The crystal structure of the title complex was determined by single crystal X-ray diffraction technique. Complex crystallized in the triclinic space group P1 with a = 0.729 08(10) nm, b= 1.020 01(14) nm, c= 1.126 28(15) nm, α = 71.644(2) °, β = 80.437(2) °, γ = 89.160(2)°, V= 0.78328(18) nm³, Z= 2, D_c= 1.547 Mg·m^-3, μ(MoKα) = 1.417 mm^-1, F(000) = 374. The final R₁ = 0.030 6, wR₂= 0.084 2 for 2 992 observed reflections [I≥2σ(I)] out of 3357 unique reflections. In this complex, copper(Ⅱ) ion is square-pyramidally coordinated by two oxygen atoms and one nitrogen atom of tridentate C₁₀H₈N₂O₃^2- ligand, one nitrogen atom of the pyridine ligand, and one oxygen atom of water molecule with the oxygen atom of water molecule locating at the apical position. The analysis of the crystal structure indicates that the complex has a one-dimensional chain structure, which is formed by intermolecular hydrogen bonds. CCDC: 222656.     

具有N…Cu作用的一维链状配合物Cu(C8H9N2O2)2的合成和晶体结构

The title complex Cu(L)₂ (HL=o-vanillin hydrazone) was synthesized by the reaction of Cu(CH₃COO)₂·H₂O with o-vanillin hydrazone in the ethanol. It was characterized by elemental analysis, IR and X-ray single crystal structure analysis. The crystal of the title complex [Cu(C₈H₉N₂O₂)₂] belongs to triclinic, space group P1 with a=0.457 57(8) nm, b=1.333 2(2) nm, c=1.386 0(3) nm, α=108.955(2)°, β=90.868(2)°, γ=95.859(2)°, V=0.794 4(2) nm³, Z=2, D_c=1.647 Mg·m^-3, μ=1.406 mm^-1, F(000)=406, and final R₁=0.035 1, wR₂=0.096 3. The complex comprises a four-coordinated copper(Ⅱ) center, with an N₂O₂ planar coordination environment. The molecules are packed in one-dimensional chain polymer though the N…Cu interaction from adjacent molecules, respectively. CCDC: 634854.     

二聚体配合物[(n-Bu)2Sn(C10H8N2O3)(C2H5OH)]2的合成和晶体结构

The novel seven-coordinate complex [(n-Bu)₂Sn(C₁₀H₈N₂O₃)(C₂H₅OH)]₂ (C₁₀H₈N₂O₃^2- is the dinegative ion of 2-oxo-propionic acid benzoyl hydrazone) was synthesized by the reaction of (n-Bu)₂SnO with 2-oxo-propionic acid benzoyl hydrazone in 1∶1 molar ratio in benzene-ethanol (V/V, 3/1), and its structure was characterized by X-ray single crystal diffraction. The crystal belongs to a tetragonal system with space group I4₁/a, a=2.4890(2)nm, b=2.4890(2)nm, c=1.5170(3)nm, V=9.398(2)nm³, Z=8, F(000)=3968, D_c=1.366g·cm^-3, and the structure was refined to final R₁=0.0530, wR₂=0.0971. The structure of the title complex is described as a dimer through weak interactions of Sn…O bonding and hydrogen bond. The tin atoms rendered sev-en-coordination in a distorted pentagonal bipyramid geometry structure, four oxygen atoms [O1, O2, O2^#1 and O4] and one nitrogen atom N2 formed the equatorial plane and C11-Sn1-C15 is the axis. CCDC: 212696.     

弱桥联二聚体丙酮酸异烟酰腙合锡(Ⅳ)配合物[(p-CNC6H4CH2)2Sn(C9H7N3O3)(H2O)]2的合成、表征和晶体结构

Diorganotin(Ⅳ) compound [(p-CNC₆H₄CH₂)₂Sn(C₉H₇N₃O₃)(H₂O)]₂ was synthesized by the reaction of tri-p-cyanobenzyltin chloride with Schiff base ligand pyruvic acid isonicotinyl hydrazone. The compound was characterized by elemental analysis, IR, ¹H NMR. The crystal structure was determined by X-ray single crystal diffraction. The crystal belongs to monoclinic space group C2/c, with a=3.143 1(3) nm, b=0.989 99(10) nm, c=1.785 68(18) nm, β=114.908 0(13)°, V=5.039 6(9) nm³, Z=4, μ=1.054 mm^-1, D_c=1.513 Mg·m^-3, F(000)=2 304, R=0.042 8, wR=0.090 3, GOF=0.997. In this compound, the Sn atom exists in a distorted octahedral coordination environment in which one water molecule, one tridentate pyruvic acid isonicotinyl hydrazone ligand, and two trans p-cyanobenzyl groups coordinate to each Sn center, the angle of the axial C10-Sn1-C18 is 166.1(2)°. Two molecules form a weak-bridged dimmer with weak interactions of Sn…O bonding and hydrogen bonds. CCDC: 270796.     

配合物Cu(C15H12N2O3)(C5H5N)的合成和晶体结构

The title coordination compound with N-substituted-salicyl Schiff ligand, Cu(C₁₅H₁₂N₂O₃)(C₅H₅N), has been synthesized. The coordination compound crystallizes in orthorhombic system, space group Pbca with a=2.037 62(7) nm, b=0.698 45(2)nm, c=2.508 76(9)nm, V=3.570 4(2) nm³, Z=8, F(000)=1 688, D_c=1.529 g·cm^-3, M_r=410.91, μ=1.250 mm^-1, R=0.031 3 and wR=0.077 0. In the coordination compound, one phenolate oxygen, one carbonyl oxygen and one hydrazine nitrogen atom from the dianionic ligand N-salicylaldehyde-N′-(4-methoxybenzoyl) hydrazone and one pyridine nitrogen atom coordinate to Cu(Ⅱ) ion, forming a distorted square plane. CCDC: 218182.     

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.     

配合物[Mn(C13H8N2OBr)2(C5H5N)2]·3C5H5N的结构与磁性研究

The complex [Mn(C₁₃H₈N₂OBr)₂(C₅H₅N)₂]·3C₅H₅N has been synthesized and characterized by X-Ray diffraction, IR and variable temperature (～10 to ～278K) magnetic susceptibility. X-Ray diffraction result for the single crystal shows that the crystal belongs to monoclinic, space group P2₁/c, a=1.0969(3)nm, b=2.0903(5)nm, c=2.0481(6)nm, β=97.366(6), V=4.657(2)nm³, Z=4, D_c=1.47g·cm^-3。     

有机-无机复合物[H2(PW12O40){Zn(C10H8N2)2(H2O)}]·1.5[Zn(C10H8N2)3]·1.75H2O的合成、结构及性能

An organic-inorganic hybrid complex, [H₂(PW₁₂O₄₀){Zn(C₁₀H₈N₂)₂(H₂O)}]·1.5[Zn(C₁₀H₈N₂)₃]·1.75H₂O has been synthesized hydrothermally and structurally characterized by X-ray crystallography. The crystal belongs to monoclinic, space grounp C2/c, with a=4.709 4(2) nm, b=1.431 77(7) nm, c=2.621 07(1) nm, β=90.125(4)°, V=17.673 4(2) nm³, Z=8, D_c=3.087 Mg·m^-3, F(000)=14 884, μ(Mo Kα)=16.327 mm^-1. The structure was refined to R₁=0.068 7 and wR₂=0.158 0 for 20 128 observed reflections with I>2σ(I). Single crystal structure shows that the title compound is constructed from [PW₁₂O₄₀]^3- cluster anion and [Zn(C₁₀H₈N₂)₂(H₂O)]²⁺ metal-organic complex cation, in which metal Zn(Ⅱ) cation are coordinately bonded to the terminal oxygen of Keggin polyanions. The title compound exhibits good catalytic activity for oxidation of benzaldehyde to benzoic acid. CCDC: 624772.     

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.     

一维链状铽配位聚合物{[Tb(p-MBA)2(H2O)2]2·(4，4′-bipy)2}n的合成、晶体结构及荧光分析

A novel one-dimensional chain coordination polymer of terbium(Ⅲ) with p-methylbenzoic acid, 2,2′-bi-pyridine and 4,4′-bipyridine has been synthesized and characterized. The crystal data of this complex C₃₉H₃₇N₃O₈Tb are as follows: monoclinic system, space group P2₁/n, a=0.974 01(10) nm, b=2.605 8(3) nm, c=1.457 77(14) nm, β=96.108(2)°, V=3.678 9(6) nm³, D_c=1.507 g·cm^-3, M_r=834.64, Z=4, μ(Mo Kα)=1.978 mm^-1, F(000)=1 684, R₁=0.032 4, wR₂=0.063 4. The crystal structure of the complex shows that the terbium(Ⅲ) ion is coordinated with eight oxygen atoms, six from five p-methylbenzoic acid molecules and two from two water molecules, respectively, forming the distorted tetraprism geometry. The luminescent property of the complex is also studied. CCDC: 619216.     

三维异核Mn-Na配合物[MnNa(N3)4(C5H5N)4]的合成与表征

Azide-containing coordination polymers have received considerable attention for the construction of new molecule-based magnets. A three dimensional heteronuclear Mn-Na compound [MnNa(N₃)₄(C₅H₅N)₄] was obtained by reaction of [Mn₃O(O₂CCH₃)₆(py)₃]ClO₄ and NaN₃ in pyridine solvents. The title compound crystallizes in monoclinic space group C2/c, a=1.536 6(2), b=1.045 3(2), c=1.576 3(2) nm, β=90.309(3)°, V=2.531 8(6) nm³, Z=4. In the structure, each Mn³⁺ and Na⁺ ion coordinated with four N atoms from four N₃^- and two N atoms from two pyridine molecules. Each pair of Mn³⁺ and Na⁺ ion are linked by N₃^- bridges into a 3D polymer with PtS topology. CCDC: 706250.     

配合物Cu(C14H10N2O2)(C5H5N)的合成和晶体结构

The novel copper(Ⅱ) complex with salicylaldehyde benzoylhydrazone and pyridine ligands， Cu(C₁₄H₁₀N₂O₂)(C₅H₅N)， has been synthesized and characterized by elemental analysis， IR and thermal analysis. The crystal structure of the title complex has been determined by single crystal X-ray diffraction techniques. The crystal belongs to monoclinic with space group P2₁/c. The cell parameters are： a=1.6362(9)nm， b=1.7140(9)nm， c=1.2255(7)nm， β=105.168(9)°， V=3.317(3)nm³， Z=8， D_c=1.525g·cm^-3， μ(MoKα)=1.334mm^-1， F(000)=1560. The structure was refined to final R₁=0.0376， wR₂=0.0909. The copper(Ⅱ) ion lies in a dis-torted square-planar environment composed of two oxygen atoms， one nitrogen atom of tridentate acyhydrazone Schiff base ligand and one nitrogen atom of the pyridine ligand. CCDC： 193111.     

二维铅配合物[Pb2(C8H4O4)2(C19H12N4O)2]n·3.5nH2O的水热合成、晶体结构与荧光性质研究

In the title compound, [Pb₂(C₈H₄O₄)₂(C₁₉H₁₂N₄O)₂]_n·3.5nH₂O(1), has been synthesized by the hydrothermal assembly of 1,4-benzenedicarboxylate and 4-(1H-1,3,7,8-tetraazacyclopenta[l]-phenanthren-2-yl)phenol(TCPP) with lead acetate. Elemental analysis, X-ray crystal structure analysis, IR spectrum, thermogravimetric analysis and luminescence property were carried out for the structural determination and characterization of the title compound. Compound 1 crystallizes in triclinic, space group P1 with a=1.013 54(10) nm, b=1.104 84(11) nm, c=1.210 05(12) nm, α=76.812 0(10)°, β=74.814 0(10)°, γ=86.030 0(10)°, V=1.273 1(2) nm³, Pb₂C₅₄H₃₉N₈O_13.5, M_r=1 430.31, Z=1, D_c=1.866 g·cm^-3, μ=6.680 mm^-1, F(000)=691, R=0.027 3 and wR=0.068 7 for 4 042 observed reflections (I>2σ(I)). The compound 1 exhibits two-dimensional network structures, which are further stacked through π-π interactions and hydrogen bonds to form three-dimensional supramolecular polymer. Solid-state luminescent spectrum of the compound 1 indicates intense fluorescent emission. CCDC: 748883.     

梯形结构有机锡配合物{[(p-MeC6H4CH2)2Sn]2(O)(Cl)OC2H5}2的合成和晶体结构

The title compound {[(p-MeC₆H₄CH₂)₂Sn]₂(O)(Cl)OC₂H₅}₂ was synthesized by the reaction of bis(p-met-hylbenzyl)tin dichloride with KOH in ethanol. The crystal structure of the complex has been determined by X- ray diffraction. The crystal belongs to monoclinic, space group P2₁/c with a=1.114 0(19) nm, b=2.423 1(3) nm, c=2.521 1(3) nm, β=99.398(3)°, V=6.714(16) nm³, Z=4, D_c=1.493 g·cm^-3, μ(Mo Kα)=15.94 cm^-1, F(000)=3 024, R₁=0.049 9, wR=0.101 7. The crystal structure shows that the coordination geometry of tin is a distorted trigonal bipyramid, and the ladder-like structure is shaped by three Sn₂O₂ planar four-membered rings. CCDC: 639682.     

配合物Ni(C14H10N2O3)(C5H5N)的合成和晶体结构

A novel nickel(Ⅱ) complex with 2,4-dihydroxybenzalidene benzoylhydrazone and pyridine ligands, Ni(C₁₄H₁₀N₂O₃)(C₅H₅N), has been synthesized and characterized by elemental analysis and IR. The crystal structure of the title complex has been determined by single crystal X-ray diffraction techniques. The crystal belongs to orthorhombic, space group Pbca. The cell parameters are: a=1.580 20(19) nm, b=1.362 18(16) nm, c=1.616 50(19) nm, and V=3.479 5(7) nm³, Z=8, D_c=1.497 Mg·m^-3, μ(MoKα)=1.139 mm^-1, F(000)=1 616, R=0.032 9 and wR=0.077 0 for 2 772 observed reflections (I>2σ(I)) out of 3810 unique ones. The nickel(Ⅱ) ion lies in a distorted square-planar environment composed of two oxygen atoms, one nitrogen atom of tridentate acyhydrazone schiff base ligand and one nitrogen atom of the pyridine ligand. The analysis of the crystal structure indicates that the complex has a one-dimensional chain structure, which is formed by intermolecular hydrogen bonds. CCDC: 244668.     

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.     

混配配合物[Zn(CF3COO)2(C7H6NS)2]的合成、晶体结构及表征

A mixed complex [Zn(CF₃COO)₂(C₇H₆NS)₂] was synthesized based on the reaction of Zn(CF₃COO)₂ and 2-aminobenzothiazol (C₇H₆NS) in methanol. The structure of the complex was characterized by elemental analysis, IR, ¹H NMR and thermal analysis. The crystal structure of the complex was determined by X-ray single crystal diffraction. The crystal belongs to monoclinic system with space group C2/c, a=3.174 3(9) nm, b=1.010 0(3) nm, c=1.723 1(5) nm, β=118.841(4)°, V=4.839(2) nm³; D_c=1.625 g·cm^-3; Z=8; F(000)=2 368; μ=1.266 mm^-1. CCDC: 600233.     

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.     

一种新颖有机-无机杂化配位聚合物[(C10H16N)2（Pb2I6）·2DMF·H2O]n的自组装合成和晶体结构(英)

A novel coordination polymer [(C₁₀H₁₆N)₂（Pb₂I₆）·2DMF·H₂O]_n (C₁₀H₁₆N=N-butyl-2-Methy-Pyridinium) was synthesized by the reaction of Pb(NO₃)₂ with C₆H₁₀NI at room temperature in DMF solvent and structurally characterized by means of X-ray single diffraction. The title compound crystallizes in triclinic system, space group P1 with a=1.1237(2) nm, b=1.25330(16) nm, c=0.808 00(12) nm, α=102.523(4)°, β=92.475(5)°, γ=95.712(10)°, V=1.102 9(3) nm³, Z=1, D_c=2.470 Mg·m^-3, F(000)=738, chemical formula C₂₆H₄₈N₄O₃Pb₂I₆ and M_r=1 640.46, μ（MoKα）=11.849 mm^-1, the final R=0.057 8 and wR=0.166 5 for 3716 observed reflections with I > 2σ(I). The title compound consists of cations ([(C₁₀H₁₆N)⁺] and anion chain(PbI₃^-),they are combined by static attracting forces in the crystal. DMF and H₂O locate between the organic and inorganic moiety. CCDC: 210812.     

[(NH2CH2CH2NH3)2WⅥO2(NHC6H4NH)2]2(NH2CH2CH2NH2)·H2O配合物的合成与晶体结构

Cis-dioxo-tungsten(Ⅵ) complex, (NH₂CH₂CH₂NH₂)[(NH₂CH₂CH₂NH₃)₂W^ⅥO₂(NHC₆H₄NH)₂]₂·H₂O is synthesized at room temperature by the reaction of sodium tungstate with o-phenylenediamine. The crystal structure of complex was determined by X-ray diffraction structural analysis. The results show that complex belongs to monoclinic system with space group P2₁/ c, a=0.712 8(2) nm, b=3.081 1(10) nm, c=0.981 9(3) nm, β=102.615(4)°, V=2.104 4(11) nm³, Z=2, μ=55.26 cm^-1, F(000)=1 176. Compared the complex with its analogous biomimetic complexes of the cofactor of molybdoenzymes and tungstoenzymses, it is found that the variance of the coordination atoms and the metal ions center have no influence on the coordination feature, and exhibits distored octahedral coordination with cis-dioxo o-phenylenediamine. CCDC: 252834.