Synthesis and Crystal Structure of a Copper(Ⅱ)Complex with Funnel-like Ligand Based on Calix[6]arene

The preparation method of a funnel like ligand derived from calix[6]arene and tris(2-pyridyl-methyl)anime has been improved.The Cu(Ⅱ)complex was obtained and ch...     

Synthesis, Structure and Thermochromic Properties of a Copper(Ⅱ) Complex Based on Naphthyl Carboxylate and Benzimidazolyl Ligands

One novel copper(Ⅱ) complex, [Cu(NAA)2(bim)2]·H2O (1, HNAA = a-naphthylacetic acid, bim = benzimidazole) has been synthesized and characterized by X-ray single-crystal diffraction analysis, elemental analysis, and IR spectrum. It crystallizes in monoclinic, space group C2/c with a = 1.15969(12), b = 1.9757(2), c = 1.45763(16) nm, β = 104.712(2)°, V = 3.2298(6) nm3, Z = 4, C38H32N4O5Cu, Mr = 688.22, Dc = 1.418 g/cm-3, μ = 0.729 mm-1, S = 1.039, F(000) = 1428, the final R = 0.0380 and wR = 0.0912 for 2849 unique reflections. In 1, two carboxylate and two benzimidazole ligands coordinate to the central Cu(Ⅱ) atom by a bidentate chelate mode. Interesting, reversible thermochromic properties of 1 can be observed and investigated by thermal analysis method.     

Synthesis and Crystal Structure of a Novel Binuclear Copper(Ⅱ)Complex,[Cu(paba)C1]

A novel binuclear Cu(Ⅱ)complex[Cu(paba)C1](pabaH=2-(2-pyridylmethylimine)benzenesulfonic acid)has been synthesized and characterized by elemental analysis,IR andsingle-crystal X-ray diffraction.The crystal of the title complex crystallizes in a monoclinie system,space group P21/n,with a=6.8165(7),b=15.3073(16),c=12.3795(13)(A),β=95.0160(10)°,V=1286.8(2)(A)3,Mr=360.26,Dc=1.860 g/cm3,μ=2.074 mm-1,F(000)=724,Z=4,the final R=0.0252 and wR=0.0675 for 2395 observed reflections with I＞2σ(I).The title complex is centrosymmetric and a pair of chlorides act as μ2-bridges to link two Cu(Ⅱ)ions forming a binuclear complex.Every Cu(Ⅱ)ion is five-coordinated by pyridyl N,imine N and sulfonate O atoms of the tridentate paba ligand as well as two bridging Cl-,constructing the distorted square-pyramidal geometry.In the structure extensive hydrogen bonds and weak π-π stacking stabilize the solid structures,through which the complex builds its 3-dimensional supramolecular structure.     

Synthesis and Crystal Structure of a Novel Binuclear Copper（Ⅱ） Complex, [Cu（paba）Cl]

A novel binuclear Cu（Ⅱ） complex [Cu（paba）Cl] （pabaH = 2-（2-pyridylmethylimine）benzenesulfonic acid） has been synthesized and characterized by elemental analysis, IR and single-crystal X-ray diffraction. The crystal of the title complex crystallizes in a monoclinic system, space group P21/n, with a = 6.8165（7）, b = 15.3073（16）, c = 12.3795（13） A^°, β= 95.0160（10）°, V= 1286.8（2） A^°^3, Mr = 360.26, Dc= 1.860 g/cm^3,μ = 2.074 mm^-1, F（000） = 724, Z = 4, the final R = 0.0252 and wR = 0.0675 for 2395 observed reflections with I 〉 20（I）. The title complex is centrosymmetric and a pair of chlorides act as μ2-bridges to link two Cu（Ⅱ） ions forming a binuclear complex. Every Cu（Ⅱ） ion is five-coordinated by pyridyl N, imine N and sulfonate O atoms of the tridentate paba ligand as well as two bridging Cl^-, constructing the distorted square-pyramidal geometry. In the structure extensive hydrogen bonds and weak π-π stacking stabilize the solid structures, through which the complex builds its 3-dimensional supramolecular structure.     

Synthesis and Crystal Structure of a Novel Copper (II) Complex with Acetylenedicarboxylate and 2, 2′-Bipyridine

The construction of molecular-based crystalline solids using coordination polymer has become a very active research field in recent years,not only due to their intriguing structural motifs,but also due to their potential applications in optical,electronic and magnetic materials1,2.Many of the most interesting coordination polymers are based on polycarboxylate ligands,such as maleate3,malonate4,1,4-benzenedicarboxylate5,1,3,5-benzenetricar-boxylate6and1,2,4,5-benzenetetracarboxylate7,which have …     

Synthesis and Crystal Structure of a Novel Terpyridine-based Cd(Ⅱ) Complex

A novel terpyridine-based complex CdL'S2 (L'= oxide of L; L = 10-hexyl-3-(2,6-di(pyridine-2-yl)pyridine-4-yl)-10H-phenothiazine) has been solvothermally synthesized and characterized by FT-IR spectroscopy, elemental analysis, 1 H NMR and X-ray crystallography. The sulfur of phenothiazine moiety was oxidized when the crystal is formed. The complex C36H37CdN5O2S3 crystallizes in triclinic, space group P1 with a = 9.4452(9), b = 13.0181(14), c = 14.6721(18), α = 73.872(1), β = 81.531(1), γ = 87.547(2)°, V = 1714.2(3)3 , Mr = 780.29, Dc = 1.512 g·cm-3 , μ = 0.861 mm-1 , F(000) = 800, Z = 2, the final R = 0.0456 and wR = 0.1059 for Ⅰ > 2σ(Ⅰ). The Cd(Ⅱ) is coordinated by two terminal sulfur ions and three pyridyl nitrogen atoms in a distorted trigonal bipyramidal geometry. Universal hydrogen bonds between the neighboring molecules have generated a supramolecular arrangement which contributes to the stability of the title complex. Fluorescence property and thermogravimetry of the complex have also been investigated and discussed.     

Synthesis,Crystal Structure and Redox Property of a Copper(Ⅱ) Complex Based on 1,1-Bis(1H-benzoimidazol-2-ylmethyl)cyclohexane

A novel mononuclear copper(Ⅱ) complex [Cu(bbmc)Cl_2]·DMF,where bbmc is 1,1-bis(1H-benzoimidazol-2-ylmethyl)cyclohexane,was synthesized and characterized by X-ray single-crystal structure analysis.The complex crystallizes in triclinic,space group P1 with a = 9.1088(5),b = 11.0075(4),c = 14.2326(6) ?,α = 97.188(3),β = 96.394(4),γ = 111.430(4)°,V = 1298.73(10) ?~3,Z = 2,D_c = 1.409 g/cm~3,μ(Mo Kα) = 1.074 mm~(-1),F(000) = 572,S = 1.078,R = 0.0381 and w R = 0.0876 for 5593 observed reflections with I 2σ(I).The central Cu(Ⅱ) ion adopts a distorted tetrahedral geometry coordinated by two nitrogen atoms of the ligand and two chloride ions.The complex showed its thermal decomposition temperature up to 226 ℃ and exhibited an irreversible one-electron transfer process involving Cu~(Ⅱ)/Cu~I couple.     

Synthesis,Structure and Photophysical Properties of a Dinuclear Copper (Ⅰ) Complex Based on Phosphinopyridine and Diphosphine Mixed-ligands

Treatment of bis(diphenylphosphino)methane(dppm)and 2-(diphenylphosphanyl)pyridine(dpppy)with Cu(CH₃CN)₄BF₄afforded a dinuclear Cu(I)complex[Cu₂(dpppy)₂(dppm)(CH₃CN)](BF₄)₂·3CH₂Cl₂(1).Complex 1 was structurally characterized by X-ray single-crystal analysis and its photophysical properties were studied in detail.It crystallizes in triclinic space group P1^-with a=13.0834(8),b=13.5568(8),c=21.8544(11)?,α=76.090(5)°,β=80.803(5)°,γ=64.582(6)°,V=3391.3(3)?³,Z=2,M_r=1507.42,D_c=1.476 g/cm³,F(000)=1532,GOOF=1.071,the final R=0.0700 for 9041 observed reflections with I>2σ(I)and wR=0.2063 for all data.The complex contains a Cu₂-core structure surrounded by one dppm and two dpppy ligands in a head-to-head arrangement.In the crystalline phase,complex 1 exhibits bright bluish-green photoluminescence(λ_max=488 nm)with high quantum yield(?=0.57)at room temperature.It is still a relatively high emission quantum yield(?=0.36)in doped PMMA thin film with 20 wt%dopant of complex 1.The emission peaks of 1 in dichloromethane solution and doped PMMA(20 wt%)thin films are 510 and 494 nm,respectively,showing a very slight bathochromic shift compared to that in crystalline phase.This phenomenon might be attributed to its rigid conformation that precludes the possible distortion of copper centers in the excited state.     

Synthesis,Crystal Structure,Fluorescent Property and DFT Calculations of a New Zn(Ⅱ) Complex Based on 3-(2-Pyridyl)-5-(4-pyridyl)-1H-1,2,4-triazole

A new coordination compound Zn(2,4?-bpt)2(H_2O)(1) based on the versatile ligand 2,4?-Hbpt(2,4?-Hbpt = 3-(2-pyridyl)-5-(4-pyridyl)-1H-1,2,4-triazole) was prepared by hydrothermal reactions. The structure of complex 1 has been characterized by X-ray single-crystal diffraction, elemental analysis, X-ray powder diffraction, IR spectrum analysis and thermogravimetric analysis. Single-crystal X-ray diffraction analysis indicates that the complex belongs to monoclinic system, space group C2/c with a = 23.877(3), b = 0.7483(9), c = 1.2492(2) ?, b = 92.681(2)°, V = 2230.6(4) ?3, Z = 4, Dc = 1.572 g/cm~3, m = 1.143 mm~(-1), Mr = 527.85 and F(000) = 1080. The final R = 0.0581 and w R = 0.0898 with I 2s(I). 1 is a 0D motif which is connected by hydrogen bonds to form a corrugated 1D pattern. In addition, 1 shows strong photoluminescent emissions in the solid state at room temperature which can be used as potential optical materials. Theoretical calculations based on density functional theory(DFT) were employed in order to explicate the stability and chemical reactivity of 2,4?-Hbpt with different conformations. The results indicated that conformation I is more stable and prior to coordination in the reactions.     

Synthesis, Crystal Structure and Antimicrobial Activity of a Novel Ni(Ⅱ) Complex

A new nickel(Ⅱ) complex, C34H38N8NiO4, has been prepared and charac-terized by X-ray diffraction analysis. It crystallizes in the monoclinic system, space group P21/c with a = 11.715(5), b = 12.328(5), c =11.113(5) A, β= 92.589(5)°, Z = 2, Dc = 1.411 g/cm3, μ = 0.658 mm-1, the final R = 0.0427 and wR = 0.1099 for 2229 observed reflections with Ⅰ> 2σ(Ⅰ). The complex is a centrosymmetric plane in which nickel(Ⅱ) is coordinated in a regular octahedron to the ligand phenytoin through the nitrogen atoms of ethylenediamine, imine and amine. The complex was valued for its antimicrobial activity against bacterial strands using the agar diffusion method, and found to be active against the four test bacterial organisms. Preliminary screening for antimicrobial activities showed that the title complex is quite active against standard strains of Salmonella species, Staphylococcus aureus, Bacillus pumilus and Eschierichia coli.     

Synthesis and Crystal Structure of a Novel Copper （Ⅱ） Complex with Acetylenedicarboxylate and 2, 2＇-Bipyridine

The title compound [Cu （ADC） （2, 2＇-bipy）]n （ADC = C2 （COO）2^2.） was prepared and characterized by elemental analysis, IR spectroscopy, X-ray analysis, respectively. The analysis of the crystal structure reveals that the copper atom is five-coordinated with two nitrogen atoms of 2, 2＇-bipy and three oxygen atoms of different acetylenedicarboxylate dianions. ADC as bridging ligands link the Cu （Ⅱ） ions, forming coordination polymer structure.     

Synthesis,Crystal Structure and Norbornene Polymerization of a Palladium(Ⅱ) Complex Based on Phenoxyimine Ligand

The title complex N,O-bis{2-[[(2,6-benzhydryl-4-methylphenyl)imino]-methyl]-phenol}-palladium(II)(C_(80)H_(64)N_2O_2 Pd) has been synthesized by the reaction of 2-[[(2,6-benzhydryl-4-methylphenyl)imino]-methyl]-phenol with Pd(CH_3COO)_2, and characterized by IR spectrum and elemental analysis. The spatial structure of the complex has been verified by single-crystal X-ray diffraction analysis. The compound belongs to the monoclinic system, space group P21/n with a = 13.492(3), b = 16.924(3), c = 14.135(3) ?, β = 97.84(3)°, V = 3197.4(11) ?~3, C_(80)H_(64)N_2O_2 Pd, Mr = 1191.73, Z = 2, Dc = 1.238 Mg/m~3, μ = 0.339 mm~(-1), F(000) = 1240, T = 293(2) K, the final R = 0.0593 and wR = 0.1192(I 2s(I)). The compound showed excellent catalytic activity up to 1.130 × 10~7 g of PNB(mol of Pd)~(-1)h~(-1) for the addition polymerization of norbornene by using methylaluminoxane(MAO) as a cocatalyst.     

Synthesis and Crystal Structure of Copper(Ⅱ)Complex with N-Acetoxyl-picolinamide

Using Cu(Ⅱ) as the template, a complex {[Cu2L2(H2O)2] 4H2O}n (L = N-acetoxyl- picolinamide) has been successfully synthesized and characterized by single-crystal X-ray diffrac tion. The crystal is of monoclinic, space group C2/c, with a = 24.144(5), b = 7.1622(14), c = 17.283(4) (A), C16H24Cu2N4O12, Mr = 591.47, β = 131.73(3)°, V = 2230.3(8) (A)3, Z = 4, Dc= 1.761 g/cm3, F(000) = 1208,μ = 1.978 mm-1, R = 0.0400 and wR = 0.1099. The copper (Ⅱ) ion is five coordinated with a distorted square pyramidal geometry. The complex can be viewed as a one dimensional chain structure by carboxylic bridges among copper atoms. In the complex there exist hydrogen bonding interactions to stabilize the structure.     

Hydrothermal Synthesis,Crystal structure,DFT and Application of a Dinuclear Cadmium(Ⅱ) Complex Based on NPHSNPAB

A new dinuclear cadmium(Ⅱ) complex,[Cd(NPHSNPAB)(H_2O)_2(CH_3CH_2OH)]_2(1),was synthesized by the hydrothermal reaction of N-phenyl-2-[2-hydroxyl-3-sulfo-5-nitrophenylazo]butadiene-1,3(NPHSNPAB) and Cd(NO_3)_2·4H_2O,and characterized by elemental analysis,infrared,UV-visible,fluorescence,thermal behavior and single-crystal X-ray diffraction. For this complex: C_(36)H_(42)Cd_2N_8O_(22)S_2,Mr = 1227.74,triclinic system,space group P1,a = 7.555(9),b = 12.006(14),c = 13.943(16) ?,α = 67.955(2),β = 88.573(2),γ = 77.550(2)o,V = 1142.5(2) ?~3,Z = 2,Dc = 1.784 g/cm~3,λ = 0.71073 ?,F(000) = 620,S = 1.125,R = 0.0460 and w R = 0.1159 for 3949 observed reflections with I 2(I). X-ray diffraction analysis reveals that the central Cd(Ⅱ) ion is bound by six oxygen atoms,forming a slightly distorted octahedral geometry. Density functional theory of complex 1 was studied. Noticeably,the application of 1 on metallic yarn got good effect.     

Synthesis,Crystal Structure and Magnetic Property of a Novel Cu(Ⅱ)-Fluconazole-azide Complex

The title compound formulated as Cu2(C13H11N6OF2)(N3)3CH3OH was synthesized and structurally characterized by elemental analysis,IR and single-crystal X-ray diffraction.In the structure of the complex,the deprotonated fluconazole and azide anion link two copper centers to construct a binuclear SBU and the azide anion exhibits a μ1,1-coordination mode.Each triazole group of fluconazole links two SBUs and the compound exhibits a chain-like architecture with strong antiferromagnetism.     

Studies on the Crystal Structure and Photoluminescence of a Mercury(Ⅱ)Complex Based on a Novel Pyridine Ligand

<正>A novel mercury(n)complex HgL_2Br_2 was prepared from HgBr_2 and the organic ligand 2-(N-methyl-N-(4-((E)-2-(pyridine-4-yl)vinyl)phenyl)amino)ethanol(L).The ligand was synthesized and then characterized by FT-IR spectroscopy,~1H NMR,mass spectrum and elemental analysis,while the single-crystal diffraction data of the complex were collected on a Siemens Smart CCD diffractometer.The complex crystallizes in triclinic space group P_1~-with a=5.367(5),b= 12.466(5),c=23.945(5)(?),α=90.812(5),β=96.318(4),γ=96.093(5)°,Z=2,D_c=1.817g·cm~(-3),μ=7.395 mm~(-1),S=0.825,and the final R=0.0396.The Hg(Ⅱ)ion in the distorted tetrahedral mercury(Ⅱ)complex C_(32)H_(36)HgBr_2N_4O_2 is coordinated by two N atoms from the two ligands together with two bromide ions.Solid-state emission of the ligand and its complex has been investigated at room temperature.     

Hydrothermal Synthesis,Crystal Structure and Fluorescent Property of a Cd(Ⅱ) Complex Based on Biimidazole and Isonicotinate-N-oxide

A new complex [Cd(H2biim)2(H2O)2]·(ino)2·4H2O (H2biim = 2,2'-biimidazole, ino = isonicotinate-N-oxide) has been prepared and characterized by single-crystal X-ray diffraction analysis, IR and fluorescence spectra analysis. The crystal is of triclinic system, space group P1 with a = 7.5380(6), b = 8.0402(7), c = 13.5094(11) , α = 104.269(1), β = 93.604(1), γ = 98.349(1)°, V = 780.93(11) 3, Mr = 765.00, Dc = 1.627 g/cm3, F(000) = 390, μ = 0.776 mm-1 and Z = 1. The final R = 0.0322 and wR = 0.0825 for 7038 observed reflections with I 2σ(I) and R = 0.0341 and wR = 0.0832 for all data. The title complex exhibits an infinite chain-like structure through bridging isonicotinate-N-oxide. Strong interchain hydrogen bonds between isonicotinate-N-oxide and H2biim result in the robust 3-D supramolecular architecture. Moreover, the complex shows strong photoluminescence with emission maximum at λ = 401 nm upon λex = 330 nm.     

Synthesis,Crystal Structure and Luminescent Property of a Zn(Ⅱ) Complex Based on 4-Imidazole-carboxylate Ligand

A new complex, [Zn(L)_2](1), has been hydrothermally prepared by the reaction of ZnSO_4·7H_2O with 2-(1H-imidazol-4-yl)benzoic acid(HL) incorporating 4-imidazolyl and carboxylate functional groups, and characterized by single-crystal X-ray diffraction, elemental analysis, IR spectroscopy and powder X-ray diffraction(PXRD). Complex 1 crystallizes in monoclinic, space group C2/c with a = 9.8349(9), b = 7.4947(7), c = 24.104(2) ?, β = 92.889(2)o, V = 1774.4(3) ?~3, Z = 4, C_(20)H_(14)N_4O_4 Zn, M_r = 439.72, D_c = 1.646 g/cm~3, μ = 1.422 mm~(-1), S = 1.003, F(000) = 896, the final R = 0.0395 and wR = 0.0874 for 11386 observed reflections(I 2σ(I)). Single-crystal X-ray structural analysis reveals that complex 1 features a two-dimensional(2D) framework with 6~3-hcb topology. Moreover, the photoluminescent property of 1 was also discussed.     

Synthesis,Crystal Structure and Luminescence Properties of a Cadmium(Ⅱ) Complex Based on 2-Hydroxy-6-methylisonicotinic Acid

A new cadmium(Ⅱ) complex[Cd(Hminic)(IP)]_n(1,Hminic = 2-hydroxy-6-methylisonicotinic acid,IP = imidazo[4,5-f]-l,10-phenanthroline),has been synthesized by the reaction of a Hminic and auxiliary N-containing ligands with Cd(Ⅱ) ion under hydrothermal conditions.The complex was studied by elemental analysis,IR spectroscopy and X-ray crystallography.It is formulated as C_(20)H_(13)CdN_5O_3,crystallizes in monoclinic system,space group C2/c with α=9.6764(8),b = 26.767(2),c = 14.1332(11) A and β= 97.4510(10)°.V= 3629.7(5) A~3,Z = 8,Mr=483.75,D_c = 1.770 g/cm~3,F(000) = 1484 and μ= 1.237 mm~(-1).The final refinement gave R = 0.0309 and wR = 0.0703 for 4151 reflections with I 2σ(I).In the structure of 1,two Cd(Ⅱ) atoms are joined by a pair of μ_2-hydroxyl oxygen atoms giving rise to a dinuclear Cd(Ⅱ) unit which is bridged by Hminic linkers to form a 1D ladder-like polymer chain.The chelating ligand IP coordinated to the Cd(Ⅱ) atom,and alternately attached to both sides of the ladder-like polymer chain.Adjacent chains are further bound together by strong intermolecular hydrogen bonds and face-to-face π…πinteractions,resulting in the formation of a 3D supramolecular architecture.Furthermore,the thermal stability and luminescent properties of this complex and the free ligands have been investigated.