The most simple method for solventless synthesis of supramolecular complex of CMCR·2BPY·BZP, [CMCR = C-methylcalix[4]resorcinarene, BPY = 4,4'-bipyridine, BZP = benzophenone], is proposed. Although CMCR ...The most simple method for solventless synthesis of supramolecular complex of CMCR·2BPY·BZP, [CMCR = C-methylcalix[4]resorcinarene, BPY = 4,4'-bipyridine, BZP = benzophenone], is proposed. Although CMCR by itself is high melting point compound (above 300°C), CMCR was found to be dissolved in melt mixture of BPY and BZPeven below 120°C. In the mixture of the three components, the reaction occurs to form CMCR·2BPY·BZP supramolecular complex.展开更多
Heat shock proteins(Hsps)are a family of abundantly expressed ATP-dependent chaperone proteins.Hsp90 is an eminent member of Hsp family.Thus far,two primary functions have been described for Hsp90:first,as a regulator...Heat shock proteins(Hsps)are a family of abundantly expressed ATP-dependent chaperone proteins.Hsp90 is an eminent member of Hsp family.Thus far,two primary functions have been described for Hsp90:first,as a regulator of conformational change of some protein kinases and nuclear hormone receptors,and the other as an indispensable factor in cellular stress response.Hsp90 has an essential number of interaction proteins since it participates in almost every biological process and its importance is self-evident.Hsp90 has an inextricable relationship in the pathogenesis of cancer,especially in the proliferation and irradiation of cancer cells,thus being a notable cancer target.Since the discovery of geldanamycin,the first inhibitor of Hsp90,from the bacterial species Streptomyces hygroscopicus,even more attention has been focused toward Hsp90.Many structure-based inhibitors of Hsp90 have been designed to develop an innovative method to defeat cancer.However,already designed inhibitors have various deficiencies,such as hepatotoxicity,poor aqueous solubility,instability,and non-ideal oral bioavailability.Based on the aforementioned reasons and to achieve an optimal performance and fewer side effects,we designed a novel inhibitor of Hsp90,called FS5,and resolved the crystal structure of the Hsp90^N-FS5 complex(1.65 A°,PDB code 5XRB).Furthermore,we compared the complexes Hsp90^N,Hsp90^N-GDM,and Hsp90^N-ATP and suggest that the inhibitor FS5 may compete with ATP for binding to Hsp90,which can be regarded as a potential strategy for the development of novel cancer drugs in the future.展开更多
The crystal structure of one novel Mn(II) complex, [Mn(pmta)_3]_2[Mn(H_2O)_6]·4H_2O(1), is reported(Hpmta = 5-methyl-1-phenyl-1H-1,2,3-triazole-4-carboxylic acid). In the title compound, the asymmetric ...The crystal structure of one novel Mn(II) complex, [Mn(pmta)_3]_2[Mn(H_2O)_6]·4H_2O(1), is reported(Hpmta = 5-methyl-1-phenyl-1H-1,2,3-triazole-4-carboxylic acid). In the title compound, the asymmetric unit consists of a [Mn(pmta_)3]ˉ anion, half [Mn(H_2O)_6]^(2+) counter cation and two lattice H_2O molecules, and the intra- and intermolecular hydrogen bonds connect the complex into a supramolecular structure. The liquid-state fluorescence spectra of complex 1 have been determined. Hirshfeld surface analysis was also studied. The main intermolecular interactions in the complex are O···H and H···H contacts.展开更多
A novel polymeric zinc(II) complex {[Zn2(TIA)(H2O)3]·(NO3)}n(1, H3TIA = 5-(1H-tetrazol-5-yl)isophthalic acid) has been synthesized in mixed solvents under solvothermal conditions and characterized by ...A novel polymeric zinc(II) complex {[Zn2(TIA)(H2O)3]·(NO3)}n(1, H3TIA = 5-(1H-tetrazol-5-yl)isophthalic acid) has been synthesized in mixed solvents under solvothermal conditions and characterized by elemental analysis, IR spectroscopy and X-ray single-crystal diffraction. Complex 1 crystallizes in orthorhombic, space group Cmcm with a = 10.4210(6), b =23.3526(14), c = 6.9214(4)A, V = 1684.37(17)A^3, Z = 4, C9H4N5O(10)Zn2, Mr = 472.91, Dc = 1.865g/cm^3, F(000) = 932, λ(MoK α) = 2.909 mm^-1, R = 0.0423 and wR = 0.1287. The complex has good thermal stability and excellent photoluminescent property.展开更多
The two complexes [HgI_2L](DMF)(1) and [AgL_2](ClO_4)(CH_3CN)(2) were synthesized from the reaction of Schiff base ligand(2-acetylpyridine-p-aminobenzoylhydrazone)(L) with HgI_2 or AgClO_4 respectively. ...The two complexes [HgI_2L](DMF)(1) and [AgL_2](ClO_4)(CH_3CN)(2) were synthesized from the reaction of Schiff base ligand(2-acetylpyridine-p-aminobenzoylhydrazone)(L) with HgI_2 or AgClO_4 respectively. The compounds are characterized by ^1H NMR,FTIR and elemental analysis. The structures of the ligand and two complexes are measured via single-crystal X-ray diffraction. In these two complexes,the structures are both distorted triangular bipyramids with five-coordinated centers.展开更多
A new structure with the molecular formula [CdL]n was formed by CdSO4 with 4-carboxymethoxy phenylacetic acid (H2L) through the hydrothermal method. The complex was characterized by elemental analysis and infrared s...A new structure with the molecular formula [CdL]n was formed by CdSO4 with 4-carboxymethoxy phenylacetic acid (H2L) through the hydrothermal method. The complex was characterized by elemental analysis and infrared spectroscopy. The structure of the complex was determined by single-crystal X-ray diffraction, which is of monoclinic system, space group P21/c with a = 10.3887(2), b = 7.10710(10), c = 14.7212(2) , β = 120.6940(10)°, V = 934.65(3) 3, Dc = 2.278 g·cm-3, Z = 4, F(000) = 624, S = 1.022, the final R = 0.0187 and wR = 0.0487 for 2000 observer reflections (Ⅰ 〉 2σ(Ⅰ)). The center metal ion Cd(Ⅱ) in the complex is six-coordinated in a distorted octahedral geometry, and is connected with L ligands to form a 3D fishing net structure, which is a novel (3,6) network topology. The luminescence of the complex has been investigated, and the result reveals that it displays luminescent property in the voilet region.展开更多
With transition metal complex, a discrete cuprous iodide compound, namely, [Ni(phen)3]2Cu6I10(1, phen = 1,10-phenanthroline) has been solvothermally synthesized and structurally characterized. Single-crystal X-ray...With transition metal complex, a discrete cuprous iodide compound, namely, [Ni(phen)3]2Cu6I10(1, phen = 1,10-phenanthroline) has been solvothermally synthesized and structurally characterized. Single-crystal X-ray diffraction studies revealed that compound 1 crystallizes in triclinic space group P1(No. 2) with a = 11.2694(2), b = 12.3699(3), c = 15.0387(3) ?, α = 102.840(2), β = 105.215(2), γ = 96.388(2)°, V = 1940.04(7) ^3, Z = 1, Dc = 2.438 g·cm^-3, F(000) = 1324, R = 0.0256 and w R = 0.0555(I 〉 2σ(I)). Compound 1 features a discrete anionic moiety of [Cu6I10]^4- charge-balanced by two metal complexes of [Ni(phen)3]2+. The optical absorption edge of compound 1 was estimated to be 2.24 eV. Interestingly, nearly 95% of contaminant(crystal violet aqueous solution(CV), 50 m L, 1.0 × 10^-5 M) could be decolorized after exposure to visible light within 30 min, illustrating an impressive photocatalytic activity of compound 1. The thermal stability of 1 has also been studied.展开更多
Two novel copper complexes with methyl or trifluoro-substituted mono-β-diiminato ligands and one acetoxyl anion were synthesized and characterized by IR spectroscopy and elemental analysis for the first time. The str...Two novel copper complexes with methyl or trifluoro-substituted mono-β-diiminato ligands and one acetoxyl anion were synthesized and characterized by IR spectroscopy and elemental analysis for the first time. The structure of complex 2 bearing trifluoro substituents was further confirmed by single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group P1 with a = 7.377(4), b = 11.727(6), c = 12.913(7) ?, α = 116.569(6), β = 98.829(7), γ = 96.520(6)°, V = 966.2(8) ?3, Z = 2, Mr = 479.86, Dc = 1.649 g/cm3, F(000) = 482, μ = 1.205 mm-1, the final R = 0.0370 and w R = 0.0903 for 3430 observed reflections with I 〉 2σ(I). These mono-β-diiminato copper complexes can effectively catalyze methacrylate(MA) polymerization when activated by MMAO. The introduction of fluoro groups into the N-aryl ring of β-diiminato ligands can greatly increase the catalytic activity of copper complexes as well as the molecular weight of PMA.展开更多
A new kind of Schiff base HL(HL= 1-phenyl-3-methyl-4-(p-methylbenzoyl)-5-pyrazolone with L-Leucine methyl ester) and complexes Ni L′_2·0.75C_2H_5OH·0.25H_2O,Cu L′′2(L′ = 1-phenyl-3-methyl-4-(p-meth...A new kind of Schiff base HL(HL= 1-phenyl-3-methyl-4-(p-methylbenzoyl)-5-pyrazolone with L-Leucine methyl ester) and complexes Ni L′_2·0.75C_2H_5OH·0.25H_2O,Cu L′′2(L′ = 1-phenyl-3-methyl-4-(p-methylbenzoyl)-5-pyrazolone with L-leucine ethyl,L′′ = 1-phenyl-3-methyl-4-(p-methylbenzoyl)-5-pyrazolone with L-leucine) have been synthesized and structurally determined by X-ray diffraction. For HL: crystal structure determination indicates that there are two independent HLs with different conformations in one asymmetric unit. For complex 1: the Ni(Ⅱ) ion is six-coordinated by two carbonyl oxygen atoms from pyrazolone ring,two nitrogen atoms from different HL′ and two oxygen atoms from L-Leucine ethyl ester to form a distorted octahedral geometry. For complex 2: the Cu(Ⅱ) ion is four-coordinated by one carbonyl oxygen atom from the pyrazolone ring,one nitrogen atom from HL′′,and two different carboxylic oxygen atoms from L-leucine with the same conformation to form a distorted quadrilateral geometry.展开更多
The title complex bis{4-chloro-2-[(6-methyl-pyridin-2-ylimino)-methyl]-phenol}-palladium(Ⅱ)(C_(26)H_(20)Cl_2N_4O_2Pd) has been synthesized by the reaction of 4-chloro-2-[(6-methylpyridin- 2-ylimino)-methy...The title complex bis{4-chloro-2-[(6-methyl-pyridin-2-ylimino)-methyl]-phenol}-palladium(Ⅱ)(C_(26)H_(20)Cl_2N_4O_2Pd) has been synthesized by the reaction of 4-chloro-2-[(6-methylpyridin- 2-ylimino)-methyl]-phenol with Pd(CH_3COO)_2, and characterized by IR spectrum and elemental analysis. Single-crystal X-ray diffraction analysis results further confirmed the molecular structures. The crystal belongs to the monoclinic system, space group P2_1/c with a = 4.1324(2), b = 23.5432(16), c = 11.8943(8) A, β = 91.238(5)o, V = 1156.93(12) ?~3, C_(26)H_(20)Cl_2N_4O_2Pd, M_r = 597.76, Z = 2, D_c = 1.716 g/cm^3, μ = 1.067 mm^(-1), F(000) = 600, the final R = 0.0247 and w R = 0.0677(I 〉 2σ(I)). In the presence of methylaluminoxane(MAO), the complex exhibits excellent catalytic activities(1.737×10~7 g of PNB(mol of Pd)^(-1)·h^(-1)) in the vinyl polymerization of norbornene.展开更多
A novel zinc complex [Zn(BIB)(bdc)]n(1, BIB = 1,3-bis(imidazol-1-yl)benzene, bdc = 1,3-benzenedicarboxylate) has been synthesized in solvothermal conditions. The title complex was characterized by elemental an...A novel zinc complex [Zn(BIB)(bdc)]n(1, BIB = 1,3-bis(imidazol-1-yl)benzene, bdc = 1,3-benzenedicarboxylate) has been synthesized in solvothermal conditions. The title complex was characterized by elemental analysis, IR spectra, thermal analysis, single-crystal and powder X-ray diffraction. The result proved that the alliance of BIB and aromatic carboxylic acids is good for the diversity of getatable structure. Complex 1 crystallizes in the monoclinic system of P2/c space group with a = 11.5591(10), b = 9.6239(8), c = 33.727(3)A, β = 103.816(3)°, V = 3643.4(5) A^3, Z = 8, μ = 1.385 mm^-1, F(000) = 1792, Dc = 1.603 g/cm^3 and Mr = 439.72 g/mol. Additionally, luminescent properties of complex 1 are also investigated and it shows good fluorescence.展开更多
The title complex bis{1-{[(6-ethyl-2-pyridinyl)imino]methylenyl}-2-naphthale- nolato-N,O}-nickel(lI) (C36H32NnO2Ni) has been synthesized by the reaction of l-{[(6-ethyl-2- pyridinyl)imino]methylenyl}-2-naphtha...The title complex bis{1-{[(6-ethyl-2-pyridinyl)imino]methylenyl}-2-naphthale- nolato-N,O}-nickel(lI) (C36H32NnO2Ni) has been synthesized by the reaction of l-{[(6-ethyl-2- pyridinyl)imino]methylenyl}-2-naphthalenol with Ni(CH3COO)2·4H2O, and characterized by IR spectrum, elemental analysis and TG. The complicated space structure has been confirmed by single-crystal X-ray diffraction analysis. The crystal belongs to the monoclinic system, space group P21/c with a = 11.410(4), b = 14.382(4), c = 18.121(6) ,A, β = 97.147(6)% V= 2950.5(16)A3, C36H32N4O2Ni, Mr = 611.37, Z = 4, Dc = 1.376 g/cm3, μ = 0.698 mm-1 F(000) = 1280, the final R = 0.0519 and wR = 0.1493 (1 〉2σ(I)). This title compound was used as precatalysts for the polymerisation of norbornene. When activated with MAO, the complex exhibited excellent catalytic activity up to 1.98 × 107 g ofPNB (mol of Ni)-1 h-1 with high monomer conversion.展开更多
A novel copper(Ⅱ) complex with tert-butyl 2-[N-(tert-butyloxycarbonylmethyl)-2-picolyamino]acetate(ampy) was synthesized and structurally characterized by elemental analysis, FT-IR spectrum, electrospray ioniza...A novel copper(Ⅱ) complex with tert-butyl 2-[N-(tert-butyloxycarbonylmethyl)-2-picolyamino]acetate(ampy) was synthesized and structurally characterized by elemental analysis, FT-IR spectrum, electrospray ionization-mass spectrometry, UV-vis spectrum and single-crystal X-ray diffraction, respectively. A mononuclear copper(II) complex with ampy, [Cu(ampy)Cl2](1), was formed irrespective of the metal-to-ligand molar ratios([Cu2+]:[ampy] = 0.5:1, 1:1, and 2:1) as a single product. Complex 1 crystallizes in the orthorhombic system, space group Pbca with a = 12.343(2), b = 18.928(3), c = 20.058(4) A, V = 4686.1(14) A3, Z = 8, Dc = 1.3349(4) g/cm3, F(000) = 1920, S = 1.016, R = 0.0693 and w R = 0.1721 for 3151 observed reflections with I 〉 2σ(I). X-ray diffraction analysis reveals that the central copper(II) ion is bound by pyridyl N, tertiary amine N and carbonyl O atoms of the quadridentate ampy as well as two Cl anions, constructing a slightly distorted octahedral geometry. Complex 1 further constructs a stable 3D supramolecular architecture by intermolecular C–H…Cl hydrogen bonds. In addition, the molecular geometry was calculated by density functional theory(DFT/B3LYP) method with the basis sets(6-31+G(d,p) for H, C, N, O and Cl atoms, and LANL2 DZ for Cu atom, respectively). The calculated results show that the optimized geometrical parameters are in good agreement with the experimental data. Natural bond orbital(NBO) analysis and frontier molecular orbitals(FMOs) analysis were investigated at the same level.展开更多
A cuprous mononuclear copper complex [Cu(adpypz)CH3CNPPh3]BF4·CH2Cl2(1, adpypz = 9,9-dimethyl-10-(6-(3-phenyl-1H-pyrazol-1-yl)pyridin-2-yl)-9,10-dihydroacridine) was synthesized and characterized by Eleme...A cuprous mononuclear copper complex [Cu(adpypz)CH3CNPPh3]BF4·CH2Cl2(1, adpypz = 9,9-dimethyl-10-(6-(3-phenyl-1H-pyrazol-1-yl)pyridin-2-yl)-9,10-dihydroacridine) was synthesized and characterized by Elemental Analysis, NMR, UV-Vis and X-ray single-crystal structure analysis. It crystallizes in triclinic, space group P1 with a = 11.3388(4), b = 13.4569(4), c = 16.2561(6) ?, α = 97.154(3), β = 92.187(3), γ = 114.119(4)°, V = 2235.38(13) ?3, Z = 2, Mr = 967.12, Dc = 1.437 g/cm^3, F(000) = 996, μ = 2.62 mm^–1, GOOF = 1.031, the final R = 0.0417, and w R = 0.1024 for 8043 observed reflections with I 〉 2σ(I). The Cu(I) atoms in the complex are four-coordinated and adopt a tetrahedral coordination geometry. In the solid state, the complex exhibits bluish-green photoluminescence with emission peaks λmax = 492 nm(1), lifetimes 235 μs and quantum yields(ф = 0.279) at room temperature. The studies of varied temperature emission spectra and decay behaviours of the complex indicate that the complex displays thermally activated delayed fluorescence(TADF) at room temperature. The results of the experimental and DFT calculations suggest that the emission in the solid state originates from the ILCT excited states.展开更多
A novel phenoxyimine-based Schiff base ligand and its mononuclear complex [C(58)H(52)N2NiO2](L = 2-benzhydryl-4-dimethoxy-3,5-dimethyl-salicylaldehyde) has been synthesized and characterized by IR spectrum, elem...A novel phenoxyimine-based Schiff base ligand and its mononuclear complex [C(58)H(52)N2NiO2](L = 2-benzhydryl-4-dimethoxy-3,5-dimethyl-salicylaldehyde) has been synthesized and characterized by IR spectrum, elemental analysis, TG, WAXD spectra, ^1H NMR and ^(13)C NMR. In addition, the molecular structure has been measured by single-crystal X-ray diffraction analysis. The crystal belongs to the monoclinic system, space group P21/c with a = 14.510(6), b = 18.573(7), c = 20.961(6) A, β = 123.453(19)°, V = 4713(3)A^3, Mr = 867.73, Z = 4, Dc = 1.223 g/cm^3, μ = 0.456 mm^-1, F(000) = 1832, the final R = 0.0685 and wR = 0.1758(I 〉 2σ(I)). The complex was used as homogeneous catalysis of polymerization of norbornene, and the MAO as cocatalyst. The nickel complex exhibited good catalytic activity up to 1.913 × 10^7 g of PNB(mol of Ni)^-1h^-1,and the yields of these reactions depend on the nature of the substituent in the aromatic ring.展开更多
The synthesis,structure and luminescent property of a tetranuclear gold(Ⅰ)complex with doubly bridging diethyldithiocarbamate(Et2dtc)and 1,1-bis(diphenylphosphino)ethene((Ph2P)2C=CH2)are described.The compl...The synthesis,structure and luminescent property of a tetranuclear gold(Ⅰ)complex with doubly bridging diethyldithiocarbamate(Et2dtc)and 1,1-bis(diphenylphosphino)ethene((Ph2P)2C=CH2)are described.The complex crystallizes in monoclinic space group C2/c with a=26.785(7),b=25.654(6),c=12.277(3)A,β=106.879(5)°,V=8073(4)A^3,Z=8,C31H32Au2F6NO3P2S2Sb,Mr=1222.32,Dc=2.011 g/cm^3,F(000)=4592,Rint=0.0529,T=293(2)K,μ=8.157 mm^(-1),the final R=0.0464 and wR=0.1444 for 5804 observed reflections with I〉2σ(Ⅰ).The intramolecular and intermolecular Au¨Au distances are 2.8670(9)and 3.2367(9)A,respectively.Weak emission appears at 517 nm at room temperature in the solid state.展开更多
A new dinuclear iron(Ill) complex has been synthesized and structurally charac- terized by X-ray crystallography: [Fem2(L)(C6HsCOO)(SO4)(CH3OH)2]·CH3CN'CH3OH (1, H3L = N,N'-bis(salicylidene)q,3-di...A new dinuclear iron(Ill) complex has been synthesized and structurally charac- terized by X-ray crystallography: [Fem2(L)(C6HsCOO)(SO4)(CH3OH)2]·CH3CN'CH3OH (1, H3L = N,N'-bis(salicylidene)q,3-diamino-2-propanol). Complex 1 belongs to orthorhombic space group Pna21 with a= 11.4400(8), b = 22.9705(2), c = 12.5712(9)A, V= 3303.5(4)A3, Z= 4, F(000) = 1576, Dc= 1.531 g·cm-3, Mr= 761.36,μ = 1.007 mm-1, S = 1.014, the final R= 0.0505 and wR= 0.1018. The crystal packing is stabilized by intermolecular O-H…O hydrogen bonds, forming an extended one-dimensional chain structure. The temperature dependence of magnetic susceptibility measurement shows that antiferromagnetic interaction is propagated between the metal centers. Fit as dinuclear arrangement gave parameters ofJ= 19.7 cm-1, g = 1.89 and R2 = 0.9999.展开更多
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 compl...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)A,α = 97.188(3),β = 96.394(4),γ = 111.430(4)°,V = 1298.73(10) A^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.展开更多
A new europium(III) complex Eu(L)3(Phen)2(1) with 2-benzoylbenzoic acid(HL) and 1,10-phenanthroline(Phen) as ligands has been synthesized. Crystal data for the complex are as follows: monoclinic, space gr...A new europium(III) complex Eu(L)3(Phen)2(1) with 2-benzoylbenzoic acid(HL) and 1,10-phenanthroline(Phen) as ligands has been synthesized. Crystal data for the complex are as follows: monoclinic, space group P21/c, a = 2.2577(4), b = 1.23484(19), c = 1.8789(3) nm, β = 94.918(3)o, V = 5.2189(14) nm^3, Dc = 1.512 g/cm^3, Z = 4, μ(Mo Kα) = 1.269 mm^-1, F(000) = 2408, the final R = 0.0433 and w R = 0.1038. The Eu(III) ion is coordinated by nine atoms to give a single-capped square antiprism coordination geometry. 1 shows two intense fluorescence emission bands arising from the transitions of Eu^3+: ^5D0→^7F1(597 nm) and ^5D0→^7F2(615 nm) with an excitation wavelength of 396 nm. In addition, 1 displays antiferromagnetic property at low temperature.展开更多
A new Zn(Ⅱ) complex, [Zn(L)2(phen)(H2O)](1, HL = N-acetyl-L-phenylalanine, phen = 1,10-phenanthroline) has been synthesized and characterized by elemental analysis, IR and X-ray single-crystal diffraction a...A new Zn(Ⅱ) complex, [Zn(L)2(phen)(H2O)](1, HL = N-acetyl-L-phenylalanine, phen = 1,10-phenanthroline) has been synthesized and characterized by elemental analysis, IR and X-ray single-crystal diffraction analysis. The Zn(Ⅱ) complex belongs to monoclinic, space group P21 with a = 12.6749(13), b = 5.5965(6), c = 22.985(2) A, β = 104.296(2)°, V = 1580.0(3) A^3, Z = 2, Mr = 676.02, Dc = 1.421 μg·m^(-3), μ = 0.833 mm^-1, F(000) = 704, and the final R = 0.0460, wR = 0.0899 for 4422 observed reflections with I 〉 2σ(I). The molecules form a 1D chained structure by hydrogen bonds. The antitumor activities of Zn(Ⅱ) complex against human hepatoma SMMC-7721 cells, human lung adenocarcinoma A549 cells and human colon carcinoma WiDr cells have also been investigated.展开更多
文摘The most simple method for solventless synthesis of supramolecular complex of CMCR·2BPY·BZP, [CMCR = C-methylcalix[4]resorcinarene, BPY = 4,4'-bipyridine, BZP = benzophenone], is proposed. Although CMCR by itself is high melting point compound (above 300°C), CMCR was found to be dissolved in melt mixture of BPY and BZPeven below 120°C. In the mixture of the three components, the reaction occurs to form CMCR·2BPY·BZP supramolecular complex.
基金supported by the Open Project of Key Laboratory of Prevention and Treatment of Cardiovascular and Cerebrovascular Diseases,Ministry of Education(No.XN201904)Gannan Medical University(No.QD201910)+1 种基金the National Natural Science Foundation of China(Nos.31770795 and 31971043)the Jiangxi Province Natural Science Foundation(No.20181ACB20014)
文摘Heat shock proteins(Hsps)are a family of abundantly expressed ATP-dependent chaperone proteins.Hsp90 is an eminent member of Hsp family.Thus far,two primary functions have been described for Hsp90:first,as a regulator of conformational change of some protein kinases and nuclear hormone receptors,and the other as an indispensable factor in cellular stress response.Hsp90 has an essential number of interaction proteins since it participates in almost every biological process and its importance is self-evident.Hsp90 has an inextricable relationship in the pathogenesis of cancer,especially in the proliferation and irradiation of cancer cells,thus being a notable cancer target.Since the discovery of geldanamycin,the first inhibitor of Hsp90,from the bacterial species Streptomyces hygroscopicus,even more attention has been focused toward Hsp90.Many structure-based inhibitors of Hsp90 have been designed to develop an innovative method to defeat cancer.However,already designed inhibitors have various deficiencies,such as hepatotoxicity,poor aqueous solubility,instability,and non-ideal oral bioavailability.Based on the aforementioned reasons and to achieve an optimal performance and fewer side effects,we designed a novel inhibitor of Hsp90,called FS5,and resolved the crystal structure of the Hsp90^N-FS5 complex(1.65 A°,PDB code 5XRB).Furthermore,we compared the complexes Hsp90^N,Hsp90^N-GDM,and Hsp90^N-ATP and suggest that the inhibitor FS5 may compete with ATP for binding to Hsp90,which can be regarded as a potential strategy for the development of novel cancer drugs in the future.
基金supported by the National Natural Science Foundation of China(No.20801012)New Energy Technology Co.Ltd.of Ai Naji of Jiangsu Province(No.8507040091)
文摘The crystal structure of one novel Mn(II) complex, [Mn(pmta)_3]_2[Mn(H_2O)_6]·4H_2O(1), is reported(Hpmta = 5-methyl-1-phenyl-1H-1,2,3-triazole-4-carboxylic acid). In the title compound, the asymmetric unit consists of a [Mn(pmta_)3]ˉ anion, half [Mn(H_2O)_6]^(2+) counter cation and two lattice H_2O molecules, and the intra- and intermolecular hydrogen bonds connect the complex into a supramolecular structure. The liquid-state fluorescence spectra of complex 1 have been determined. Hirshfeld surface analysis was also studied. The main intermolecular interactions in the complex are O···H and H···H contacts.
基金Supported by the National Natural Science Foundation of China(No.21576112)the Program for New Century Excellent Talents in University(NCET-10-0176)of ChinaNatural Science Foundation Project of Jilin Province(No.20130521019JH and 201215219)
文摘A novel polymeric zinc(II) complex {[Zn2(TIA)(H2O)3]·(NO3)}n(1, H3TIA = 5-(1H-tetrazol-5-yl)isophthalic acid) has been synthesized in mixed solvents under solvothermal conditions and characterized by elemental analysis, IR spectroscopy and X-ray single-crystal diffraction. Complex 1 crystallizes in orthorhombic, space group Cmcm with a = 10.4210(6), b =23.3526(14), c = 6.9214(4)A, V = 1684.37(17)A^3, Z = 4, C9H4N5O(10)Zn2, Mr = 472.91, Dc = 1.865g/cm^3, F(000) = 932, λ(MoK α) = 2.909 mm^-1, R = 0.0423 and wR = 0.1287. The complex has good thermal stability and excellent photoluminescent property.
基金Supported by the National Natural Science Foundation of China(No.21061003)
文摘The two complexes [HgI_2L](DMF)(1) and [AgL_2](ClO_4)(CH_3CN)(2) were synthesized from the reaction of Schiff base ligand(2-acetylpyridine-p-aminobenzoylhydrazone)(L) with HgI_2 or AgClO_4 respectively. The compounds are characterized by ^1H NMR,FTIR and elemental analysis. The structures of the ligand and two complexes are measured via single-crystal X-ray diffraction. In these two complexes,the structures are both distorted triangular bipyramids with five-coordinated centers.
基金Supported by the Natural Science Foundation of Zhejiang Province (Y12B010003)
文摘A new structure with the molecular formula [CdL]n was formed by CdSO4 with 4-carboxymethoxy phenylacetic acid (H2L) through the hydrothermal method. The complex was characterized by elemental analysis and infrared spectroscopy. The structure of the complex was determined by single-crystal X-ray diffraction, which is of monoclinic system, space group P21/c with a = 10.3887(2), b = 7.10710(10), c = 14.7212(2) , β = 120.6940(10)°, V = 934.65(3) 3, Dc = 2.278 g·cm-3, Z = 4, F(000) = 624, S = 1.022, the final R = 0.0187 and wR = 0.0487 for 2000 observer reflections (Ⅰ 〉 2σ(Ⅰ)). The center metal ion Cd(Ⅱ) in the complex is six-coordinated in a distorted octahedral geometry, and is connected with L ligands to form a 3D fishing net structure, which is a novel (3,6) network topology. The luminescence of the complex has been investigated, and the result reveals that it displays luminescent property in the voilet region.
基金Supported by the NNSFC(No.21373223)Chunmiao project of Haixi Institute of Chinese Academy of Sciences(CMZX-2014-001)
文摘With transition metal complex, a discrete cuprous iodide compound, namely, [Ni(phen)3]2Cu6I10(1, phen = 1,10-phenanthroline) has been solvothermally synthesized and structurally characterized. Single-crystal X-ray diffraction studies revealed that compound 1 crystallizes in triclinic space group P1(No. 2) with a = 11.2694(2), b = 12.3699(3), c = 15.0387(3) ?, α = 102.840(2), β = 105.215(2), γ = 96.388(2)°, V = 1940.04(7) ^3, Z = 1, Dc = 2.438 g·cm^-3, F(000) = 1324, R = 0.0256 and w R = 0.0555(I 〉 2σ(I)). Compound 1 features a discrete anionic moiety of [Cu6I10]^4- charge-balanced by two metal complexes of [Ni(phen)3]2+. The optical absorption edge of compound 1 was estimated to be 2.24 eV. Interestingly, nearly 95% of contaminant(crystal violet aqueous solution(CV), 50 m L, 1.0 × 10^-5 M) could be decolorized after exposure to visible light within 30 min, illustrating an impressive photocatalytic activity of compound 1. The thermal stability of 1 has also been studied.
基金Supported by the National Natural Science Foundation of China(21172269)the Applied Fundamental Research Project of Wuhan City(2015011701011598)
文摘Two novel copper complexes with methyl or trifluoro-substituted mono-β-diiminato ligands and one acetoxyl anion were synthesized and characterized by IR spectroscopy and elemental analysis for the first time. The structure of complex 2 bearing trifluoro substituents was further confirmed by single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group P1 with a = 7.377(4), b = 11.727(6), c = 12.913(7) ?, α = 116.569(6), β = 98.829(7), γ = 96.520(6)°, V = 966.2(8) ?3, Z = 2, Mr = 479.86, Dc = 1.649 g/cm3, F(000) = 482, μ = 1.205 mm-1, the final R = 0.0370 and w R = 0.0903 for 3430 observed reflections with I 〉 2σ(I). These mono-β-diiminato copper complexes can effectively catalyze methacrylate(MA) polymerization when activated by MMAO. The introduction of fluoro groups into the N-aryl ring of β-diiminato ligands can greatly increase the catalytic activity of copper complexes as well as the molecular weight of PMA.
文摘A new kind of Schiff base HL(HL= 1-phenyl-3-methyl-4-(p-methylbenzoyl)-5-pyrazolone with L-Leucine methyl ester) and complexes Ni L′_2·0.75C_2H_5OH·0.25H_2O,Cu L′′2(L′ = 1-phenyl-3-methyl-4-(p-methylbenzoyl)-5-pyrazolone with L-leucine ethyl,L′′ = 1-phenyl-3-methyl-4-(p-methylbenzoyl)-5-pyrazolone with L-leucine) have been synthesized and structurally determined by X-ray diffraction. For HL: crystal structure determination indicates that there are two independent HLs with different conformations in one asymmetric unit. For complex 1: the Ni(Ⅱ) ion is six-coordinated by two carbonyl oxygen atoms from pyrazolone ring,two nitrogen atoms from different HL′ and two oxygen atoms from L-Leucine ethyl ester to form a distorted octahedral geometry. For complex 2: the Cu(Ⅱ) ion is four-coordinated by one carbonyl oxygen atom from the pyrazolone ring,one nitrogen atom from HL′′,and two different carboxylic oxygen atoms from L-leucine with the same conformation to form a distorted quadrilateral geometry.
基金Supported by the Ministry of Education of China(No.208066)the Education Department of Fujian Province(JA07029)the State Key Laboratory of Structural Chemistry(No.20130013)
文摘The title complex bis{4-chloro-2-[(6-methyl-pyridin-2-ylimino)-methyl]-phenol}-palladium(Ⅱ)(C_(26)H_(20)Cl_2N_4O_2Pd) has been synthesized by the reaction of 4-chloro-2-[(6-methylpyridin- 2-ylimino)-methyl]-phenol with Pd(CH_3COO)_2, and characterized by IR spectrum and elemental analysis. Single-crystal X-ray diffraction analysis results further confirmed the molecular structures. The crystal belongs to the monoclinic system, space group P2_1/c with a = 4.1324(2), b = 23.5432(16), c = 11.8943(8) A, β = 91.238(5)o, V = 1156.93(12) ?~3, C_(26)H_(20)Cl_2N_4O_2Pd, M_r = 597.76, Z = 2, D_c = 1.716 g/cm^3, μ = 1.067 mm^(-1), F(000) = 600, the final R = 0.0247 and w R = 0.0677(I 〉 2σ(I)). In the presence of methylaluminoxane(MAO), the complex exhibits excellent catalytic activities(1.737×10~7 g of PNB(mol of Pd)^(-1)·h^(-1)) in the vinyl polymerization of norbornene.
基金supported by grants from Provincial Key Projects of Anhui Natural Science Research in Universities(No.KJ2015A203)the Natural Science Foundation of Anhui Province(No.1408085MB40)Projects of Anhui Key Laboratory of Spin Electron and Nanomaterials,Suzhou University(No.2014YKF51)
文摘A novel zinc complex [Zn(BIB)(bdc)]n(1, BIB = 1,3-bis(imidazol-1-yl)benzene, bdc = 1,3-benzenedicarboxylate) has been synthesized in solvothermal conditions. The title complex was characterized by elemental analysis, IR spectra, thermal analysis, single-crystal and powder X-ray diffraction. The result proved that the alliance of BIB and aromatic carboxylic acids is good for the diversity of getatable structure. Complex 1 crystallizes in the monoclinic system of P2/c space group with a = 11.5591(10), b = 9.6239(8), c = 33.727(3)A, β = 103.816(3)°, V = 3643.4(5) A^3, Z = 8, μ = 1.385 mm^-1, F(000) = 1792, Dc = 1.603 g/cm^3 and Mr = 439.72 g/mol. Additionally, luminescent properties of complex 1 are also investigated and it shows good fluorescence.
基金Supported by the Natural Science Foundation of Fujian Province(2010J01026)the Ministry of Education of China(No.208066)+1 种基金the Education Department of Fujian Province(JA07029)the State Key Laboratory of Structural Chemistry(No.20130013)
文摘The title complex bis{1-{[(6-ethyl-2-pyridinyl)imino]methylenyl}-2-naphthale- nolato-N,O}-nickel(lI) (C36H32NnO2Ni) has been synthesized by the reaction of l-{[(6-ethyl-2- pyridinyl)imino]methylenyl}-2-naphthalenol with Ni(CH3COO)2·4H2O, and characterized by IR spectrum, elemental analysis and TG. The complicated space structure has been confirmed by single-crystal X-ray diffraction analysis. The crystal belongs to the monoclinic system, space group P21/c with a = 11.410(4), b = 14.382(4), c = 18.121(6) ,A, β = 97.147(6)% V= 2950.5(16)A3, C36H32N4O2Ni, Mr = 611.37, Z = 4, Dc = 1.376 g/cm3, μ = 0.698 mm-1 F(000) = 1280, the final R = 0.0519 and wR = 0.1493 (1 〉2σ(I)). This title compound was used as precatalysts for the polymerisation of norbornene. When activated with MAO, the complex exhibited excellent catalytic activity up to 1.98 × 107 g ofPNB (mol of Ni)-1 h-1 with high monomer conversion.
基金supported by the National Basic Research Program of China(No.2014CB643401)the National Natural Science Foundation of China(Nos.51134007 and 51474256)
文摘A novel copper(Ⅱ) complex with tert-butyl 2-[N-(tert-butyloxycarbonylmethyl)-2-picolyamino]acetate(ampy) was synthesized and structurally characterized by elemental analysis, FT-IR spectrum, electrospray ionization-mass spectrometry, UV-vis spectrum and single-crystal X-ray diffraction, respectively. A mononuclear copper(II) complex with ampy, [Cu(ampy)Cl2](1), was formed irrespective of the metal-to-ligand molar ratios([Cu2+]:[ampy] = 0.5:1, 1:1, and 2:1) as a single product. Complex 1 crystallizes in the orthorhombic system, space group Pbca with a = 12.343(2), b = 18.928(3), c = 20.058(4) A, V = 4686.1(14) A3, Z = 8, Dc = 1.3349(4) g/cm3, F(000) = 1920, S = 1.016, R = 0.0693 and w R = 0.1721 for 3151 observed reflections with I 〉 2σ(I). X-ray diffraction analysis reveals that the central copper(II) ion is bound by pyridyl N, tertiary amine N and carbonyl O atoms of the quadridentate ampy as well as two Cl anions, constructing a slightly distorted octahedral geometry. Complex 1 further constructs a stable 3D supramolecular architecture by intermolecular C–H…Cl hydrogen bonds. In addition, the molecular geometry was calculated by density functional theory(DFT/B3LYP) method with the basis sets(6-31+G(d,p) for H, C, N, O and Cl atoms, and LANL2 DZ for Cu atom, respectively). The calculated results show that the optimized geometrical parameters are in good agreement with the experimental data. Natural bond orbital(NBO) analysis and frontier molecular orbitals(FMOs) analysis were investigated at the same level.
基金supported by the National Natural Science Foundation of China(51172232)
文摘A cuprous mononuclear copper complex [Cu(adpypz)CH3CNPPh3]BF4·CH2Cl2(1, adpypz = 9,9-dimethyl-10-(6-(3-phenyl-1H-pyrazol-1-yl)pyridin-2-yl)-9,10-dihydroacridine) was synthesized and characterized by Elemental Analysis, NMR, UV-Vis and X-ray single-crystal structure analysis. It crystallizes in triclinic, space group P1 with a = 11.3388(4), b = 13.4569(4), c = 16.2561(6) ?, α = 97.154(3), β = 92.187(3), γ = 114.119(4)°, V = 2235.38(13) ?3, Z = 2, Mr = 967.12, Dc = 1.437 g/cm^3, F(000) = 996, μ = 2.62 mm^–1, GOOF = 1.031, the final R = 0.0417, and w R = 0.1024 for 8043 observed reflections with I 〉 2σ(I). The Cu(I) atoms in the complex are four-coordinated and adopt a tetrahedral coordination geometry. In the solid state, the complex exhibits bluish-green photoluminescence with emission peaks λmax = 492 nm(1), lifetimes 235 μs and quantum yields(ф = 0.279) at room temperature. The studies of varied temperature emission spectra and decay behaviours of the complex indicate that the complex displays thermally activated delayed fluorescence(TADF) at room temperature. The results of the experimental and DFT calculations suggest that the emission in the solid state originates from the ILCT excited states.
基金Supported by the Ministry of Education of China(No.208066)the Education Department of Fujian Province(JA07029)the State Key Laboratory of Structural Chemistry(No.20130013)
文摘A novel phenoxyimine-based Schiff base ligand and its mononuclear complex [C(58)H(52)N2NiO2](L = 2-benzhydryl-4-dimethoxy-3,5-dimethyl-salicylaldehyde) has been synthesized and characterized by IR spectrum, elemental analysis, TG, WAXD spectra, ^1H NMR and ^(13)C NMR. In addition, the molecular structure has been measured by single-crystal X-ray diffraction analysis. The crystal belongs to the monoclinic system, space group P21/c with a = 14.510(6), b = 18.573(7), c = 20.961(6) A, β = 123.453(19)°, V = 4713(3)A^3, Mr = 867.73, Z = 4, Dc = 1.223 g/cm^3, μ = 0.456 mm^-1, F(000) = 1832, the final R = 0.0685 and wR = 0.1758(I 〉 2σ(I)). The complex was used as homogeneous catalysis of polymerization of norbornene, and the MAO as cocatalyst. The nickel complex exhibited good catalytic activity up to 1.913 × 10^7 g of PNB(mol of Ni)^-1h^-1,and the yields of these reactions depend on the nature of the substituent in the aromatic ring.
基金financial supports from the NNSFC(20931006,U0934003,and 91122006)the NSF of Fujian Province(2011J01065)
文摘The synthesis,structure and luminescent property of a tetranuclear gold(Ⅰ)complex with doubly bridging diethyldithiocarbamate(Et2dtc)and 1,1-bis(diphenylphosphino)ethene((Ph2P)2C=CH2)are described.The complex crystallizes in monoclinic space group C2/c with a=26.785(7),b=25.654(6),c=12.277(3)A,β=106.879(5)°,V=8073(4)A^3,Z=8,C31H32Au2F6NO3P2S2Sb,Mr=1222.32,Dc=2.011 g/cm^3,F(000)=4592,Rint=0.0529,T=293(2)K,μ=8.157 mm^(-1),the final R=0.0464 and wR=0.1444 for 5804 observed reflections with I〉2σ(Ⅰ).The intramolecular and intermolecular Au¨Au distances are 2.8670(9)and 3.2367(9)A,respectively.Weak emission appears at 517 nm at room temperature in the solid state.
基金Supported by the Natural Science Foundation of Mongolian Autonomous Region,China(No.2014MS0215)
文摘A new dinuclear iron(Ill) complex has been synthesized and structurally charac- terized by X-ray crystallography: [Fem2(L)(C6HsCOO)(SO4)(CH3OH)2]·CH3CN'CH3OH (1, H3L = N,N'-bis(salicylidene)q,3-diamino-2-propanol). Complex 1 belongs to orthorhombic space group Pna21 with a= 11.4400(8), b = 22.9705(2), c = 12.5712(9)A, V= 3303.5(4)A3, Z= 4, F(000) = 1576, Dc= 1.531 g·cm-3, Mr= 761.36,μ = 1.007 mm-1, S = 1.014, the final R= 0.0505 and wR= 0.1018. The crystal packing is stabilized by intermolecular O-H…O hydrogen bonds, forming an extended one-dimensional chain structure. The temperature dependence of magnetic susceptibility measurement shows that antiferromagnetic interaction is propagated between the metal centers. Fit as dinuclear arrangement gave parameters ofJ= 19.7 cm-1, g = 1.89 and R2 = 0.9999.
基金Financially supported from National Natural Science Foundation of China(No.21403191)Natural Science Foundation of Guangdong Province(Nos.2014A030307010 and 2015A0303010406)+2 种基金Special funds for public welfare research and capacity building in Guangdong Province(No.2015A010105031)Zhanjiang Science Technology Project(No.2013B01054)Lingnan Normal University Science Research Foundation(Nos.L1301 and LZL1504)
文摘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)A,α = 97.188(3),β = 96.394(4),γ = 111.430(4)°,V = 1298.73(10) A^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.
基金Supported by the Doctoral Scientific Research Foundation of Hengyang Normal University(16D06)the Open Fund Project of Key Laboratory of Functional Organometallic Materials of Hengyang Normal University(GN15K02)
文摘A new europium(III) complex Eu(L)3(Phen)2(1) with 2-benzoylbenzoic acid(HL) and 1,10-phenanthroline(Phen) as ligands has been synthesized. Crystal data for the complex are as follows: monoclinic, space group P21/c, a = 2.2577(4), b = 1.23484(19), c = 1.8789(3) nm, β = 94.918(3)o, V = 5.2189(14) nm^3, Dc = 1.512 g/cm^3, Z = 4, μ(Mo Kα) = 1.269 mm^-1, F(000) = 2408, the final R = 0.0433 and w R = 0.1038. The Eu(III) ion is coordinated by nine atoms to give a single-capped square antiprism coordination geometry. 1 shows two intense fluorescence emission bands arising from the transitions of Eu^3+: ^5D0→^7F1(597 nm) and ^5D0→^7F2(615 nm) with an excitation wavelength of 396 nm. In addition, 1 displays antiferromagnetic property at low temperature.
基金supported by the National Natural Science Foundation of China(No.21171132)the Project of Shandong Province Higher Educational Science and Technology Program(J14LC01)Science Foundation of Weifang
文摘A new Zn(Ⅱ) complex, [Zn(L)2(phen)(H2O)](1, HL = N-acetyl-L-phenylalanine, phen = 1,10-phenanthroline) has been synthesized and characterized by elemental analysis, IR and X-ray single-crystal diffraction analysis. The Zn(Ⅱ) complex belongs to monoclinic, space group P21 with a = 12.6749(13), b = 5.5965(6), c = 22.985(2) A, β = 104.296(2)°, V = 1580.0(3) A^3, Z = 2, Mr = 676.02, Dc = 1.421 μg·m^(-3), μ = 0.833 mm^-1, F(000) = 704, and the final R = 0.0460, wR = 0.0899 for 4422 observed reflections with I 〉 2σ(I). The molecules form a 1D chained structure by hydrogen bonds. The antitumor activities of Zn(Ⅱ) complex against human hepatoma SMMC-7721 cells, human lung adenocarcinoma A549 cells and human colon carcinoma WiDr cells have also been investigated.