2′-(4-氟基苯亚甲基)-3，5-二羟基苯甲酰腙Ni(Ⅱ)配合物的合成、表征、晶体结构及光谱性质

In ethanol, a new mononuclear nickel(Ⅱ) complex incorporating Schiff base ligands, [NiL₂](DMF)₄ (HL=2′-(4-fluorobenzylidene)-3,5-dihydroxybenzoylhy drazide) has been synthesized and characterized by IR, UV-Vis, elemental analysis and X-ray crystal structure analysis. The single crystal structure has been determined by single-crystal X-ray diffraction structure analysis. The crystal belongs to monoclinic system, space group P2₁/c with a=1.617 3(2) nm,b=1.798 5(2) nm, c=0.737 61(10) nm, β=91.953(3)°, V=2.144 3(5) nm³, Z=2, μ=0.526 mm^-1, D_c=1.390 g·cm^-3, F(000)=940, R_int=0.105 3. In the compound nickel(Ⅱ) atom is four-coordinated with two nitrogen atoms from amide and two oxygen atoms from keto group. The complex has the centrosymmetry and the nickel(Ⅱ) ion is located in the center. CCDC: 675522.     

超分子钴(Ⅱ)配合物[CoL(H2O)2]n的合成与结构表征

A mononuclear Cobalt(Ⅱ) complex [CoL(H₂O)₂]_n (H₂L: 4,4′,6,6′-Tetrabromo-2,2′-[ethylenedioxybis(nitrilomethylidyne)]diphenol), has been synthesized and structurally characterized by elemental analysis, IR and X-ray diffraction single crystal structure analysis. The crystal of the complex belongs to monoclinic space group P2₁/c with a=2.516 8(3) nm, b=1.023 43(18) nm, c=0.789 17(14) nm, β=91.375(2)°, V=2.032 1(5) nm³, Z=4, D_c=2.317 Mg·m^-3, μ(Mo Kα)=8.747 mm^-1, F(000)=1 356, R₁=0.049 7, wR₂=0.110 4. The crystal structure of [CoL(H₂O)₂]_n indicates that the complex consists of one cobalt(Ⅱ) atom, one L^2- unit and two coordinated water molecules, and the coordination number of the cobalt(Ⅱ) atom is six. One-dimensional chain supramolecular structure is formed by intermolecular hydrogen bonds and π-π stacking of neighboring benzene rings. CCDC: 652649.     

Cu2(μ-dppb)2(μ-Cl)2的合成、晶体结构及非线性光学性质

The complex Cu₂(μ-dppb)₂(μ-Cl)₂ has been synthesized from the reaction of CuCl， dppb and (n-Bu)₄NCl. The crystal belongs to the triclinic with space group P1. The unit cell parameters are: a=9.939(4)?， b=10.083(6)?， c=14.104(5)?， α=76.46(3)°， β=71.02(2)°， γ=70.87(5)°. The single crystal X-ray diffraction analysis reveals that it has a bi-ring structure with a symmetry center at the middle of two Copper atoms. The outer ring is a 14-membered ring of Cu-dppb-Cu-dppb， and the inner ring is a 4-membered ring composed of two Cl^- and two Cu(Ⅰ). Investigation of third-order optical nonlinearity shows that it exhibits considerable nonlinear absorptive and self-defocusing effect with α₂=1.75×10^-13m·W^-1 and n₂=3.19×10^-18m²·W^-1. CCDC: 193113.     

牛磺酸合铜螯合物的合成及晶体结构

The new chelate complex formulated [Cu(NC₂H₆SO₃)(phen)(CH₃CO₂)]·2H₂O (phen is o-phenanthroline) has been synthesized and the crystal structure was determined by X-ray diffraction. The crystal structure of the complex belongs to triclinic system with space group and unite cell parameters： a=7.298(1)?， b=11.573(2)?， c=11.942(3)?;α=69.77(1)°， β=80.05(1)°， γ=76.39(1)°， V=915.2(3)?³， Z=2， F(000)=478. D_c=1.680g·cm^-3， μ=1.354mm^-1， S=1.045. In the crystal structure Cu(Ⅱ) ion is five-coordinated to form a distorted tragonal cone. CCDC： 193112.     

以Schiff碱N-丁酰基水杨酰肼为配体的三核镍(Ⅱ)配合物的合成与结构

The trinuclear nickel(Ⅱ) complex Ni₃(C₁₁H₁₁N₂O₃)₂(C₅H₅N)₄ was prepared by the reaction of Ni(OAc)₂·4H₂O with N-butylsalicylhydrazide Schiff base ligand and characterized by X-ray crystallography. The crystal belongs to triclinic， M_r=930.91， space group P1 with cell parameters a=9.8489(2)?， b=12.3110(2)?， c=18.4035(3)?， α=71.353(2)°， β=76.638(2)°，γ=84.815(2)°，V=2056.72(6)?³，Z=2，D_c=1.503g·cm^-3， μ(MoKα) =1.417mm^-1， F(000)=964， R=0.0317， wR=0.0868. A total of 5393 independent reflections were collected， of which 4448 reflections with I ≥ 2σ(I) were observed. There are two centrosymmetrical trin-uclear molecules in a unit cell， each molecule exhibits a linear trinuclear metal arrangement with the Ni…Ni…Ni angle of 180°. The interatomic distances between the nickel atoms on the two sides are 9.2030(8)? and 9.1876(9)? for the two molecules， respectively. The central nickel atom adopts an axially elongated octahedral geometry whereas the nickel atoms on the two sides have square-planar coordination environment. CCDC： 194083.     

[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.     

2′-(2-噻吩亚甲基)-2-羟基苯甲酰腙钴(Ⅲ)配合物的合成、表征及晶体结构

In ethanol, a mononuclear cobalt(Ⅱ) complex incorporating 2′-(2-Thienylidene)-2-Hydroxybenzoylhydra-zide has been synthesized and characterized by IR, UV-Vis, elemental analysis and X-ray crystal structure analysis. The crystal belongs to triclinic system, space group P1 with cell constant, a=1.230 69(10) nm, b=1.329 18(11) nm, c=1.330 56(11) nm, α=113.702(2)°, β=91.590(2)°, γ=100.846(2)°, V=1.944 4(3) nm³, Z=2, μ=0.662 mm^-1, D_c=1.482 g·cm^-3, F(000)=896, R_int=0.048 7. The crystal structure shows an anionic didentate ligand O and N donors in this work. The cobalt(Ⅲ) atom is hexacoordinated with oxygen atom from keto group and nitrogen atom from amide to form a cobalt atom for the core octahedral structure. CCDC: 748882.     

N-苯基亚氨基二乙酸镍二维网状配合物的合成及结构表征(英)

A new nickel(Ⅱ) coordination compound [Ni(L^2-)(2,2′-bipy)(H₂O)]·2H₂O (H₂L=phenyliminodiacetic acid) was obtained by self-assembly of phenyliminodiacetic acid, 2,2′-bipy, and NiCl₂·6H₂O in the mixed solvent of water and ethanol (V∶V=1∶1). The complex was characterized by elemental analysis, IR spectra, and X-ray crystallography analysis. The crystal is monoclinic, space group P2₁ /c with a=0.867 4(2) nm, b=0.907 3(1) nm, c=2.643 5(5) nm, β=91.01(1)°, V=2.080 2(4) nm³, Z=4, F(000)=992, D_c=1.520 Mg·m^-3, R₁=0.027 0 and wR₂=0.067 5. In the complex, nickel (Ⅱ) atom is coordinated with a distorted octahedral geometry and extensive hydrogen bonds link the complexes into a 2D network structure. CCDC: 244926.     

2D氢键网状Mg(Ⅱ)配合物的合成和晶体结构

The title complex [Mg(H₂O)₆]·(L)·(H₂O) [L=2-formyl-benzenesulfonate-hydrazine] was synthesized by the reaction of magnesium chloride hexahydrate with 2-formyl-benzenesulfonic acid sodium-hydrazine in the CH₃CH₂OH/H₂O. It was characterized by elemental analysis, IR and X-ray single crystal structure analysis. The crystal of the title complex [Mg(H₂O)₆]·(C₁₄H₁₂N₂O₇S₂)·(H₂O) belongs to triclinic, space group P1 with a=0.781 09(12) nm, b=0.781 27(13) nm, c=0.995 68(19) nm, α=102.054(2)°, β=92.331 0(10)°, γ=105.500(2)°, V=0.569 59(17) nm³, Z=1, D_c=1.559 Mg·m^-3, μ=0.334 mm^-1, F(000)=280, and final R₁=0.033 9, wR₂=0.091 6. The complex comprises a six-coordinated magnesium(Ⅱ) center, with a O₆ distorted octahedron coordination environment. The molecules are connected by hydrogen bonds to form two dimensional network structures. CCDC: 716601.     

3-乙氧基水杨醛缩N，N-双(3-胺基丙烷)-甲基氨Zn(Ⅱ)配合物的合成、晶体结构及荧光性质

The reaction of 3-ethoxysalicylaldehyde-N,N-bis(3-aminopropyl)methylamine with Zn(Ⅱ) acetate in CH₃CH₂OH followed by recrystallization in CH₃CH₂OH gave rise to colourless block crystals of 3-ethoxysali-cylaldehyde-N,N-bis(3-aminopropyl)methylamine Zn(Ⅱ). The compound has been characterized by elemental analysis, IR spectrum, molar conductivity and X-ray diffraction structure determination single crystal. It crystallizes in monoclinic, space group P2₁/c with a=1.028 91(13) nm, b=1.400 35(12) nm, c=1.733 69(19) nm, V=2.476 6(5) nm³, Z=4, M_r=504.91, D_c=1.354 g·cm^-3, T=298(2) K, F(000)=1 064, μ(Mo Kα)=0.102 7 cm-1, R=0.068 4 and wR=0.185 3 for 2 940 observed reflections with I>2σ(I). The fluorescence properties of ligand and the complex also have been investigated. The results show that the fluorescence intensity of the Zn(Ⅱ) complex is very stronger than the ligand. In the crystal, the molecules form 1D chain structure by π-π stacking. CCDC: 675010.