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1.
Two new zinc-triazole-carboxylate frameworks constructed from secondary building units (SBUs), [Zn5(trz)4(btc)2(DMF)2(H2O)2]·2H2O·DMF (1) and [Zn4(trz)3(btc)2(CH3CN)(H2O)]·5H2O·(Bu4N) (2), [Htrz = 1,2,4-triazole, H3btc = 1,2,4-benzenetricarboxylate, Bu4N = tetrabutylammonium], have been synthesized by solvothermal reactions and characterized by single-crystal X-ray diffraction analyses, X-ray power diffraction, elemental analyses, infrared spectra and thermogravimetric analyses. Both compounds 1 and 2 exhibit 3D (3,8)-connected tfz-d nets with {43}2{46.618.84} topology symbol built from rod-shaped {[Zn5(trz)4]6+}n SBUs (1) and {[Zn4(trz)3]5+}n SBUs (2). In two compounds, rodlike units are connected by btc ligands via different modes. Additionally, solid state fluorescent emission spectra of two compounds show fluorescent properties at room temperature. 相似文献
2.
A series of substituted pyrazolo[1,5-a]pyrazin-4(5H)-one was synthesized by the reaction of ethyl 1-(2-oxo-2-phenylethyl)-3-phenyl-1H-pyrazole-5-carboxylate derivatives and 2-(2-aminoethoxy)ethanol or 2-morpholinoethanamine in the condition of microwave-assisted one-step and solvent-free in a good yield. The structures of the compounds were determined by IR, 1H NMR and mass spectroscopy. In addition, a representative single-crystal structure was characterized by using X-ray diffraction analysis. Preliminary biological evaluation showed that the compounds could inhibit the growth of A549 and H322 cells in dosage-dependent manners. 相似文献
3.
Ten limonoids, named godavarins A-J (1-7, 9-11), were isolated from seeds of an Indian mangrove (Xylocarpus moluccensis) collected in the mangrove wetlands of Godavari estuary, Andhra Pradesh. Eight known limonoids, viz. xyloccensins L (8), P (12), Q (13), mexicanolide (14), 6-deoxy-3-detigloyl-swietenine acetate (15), fissinolide (16), methyl 3β-acetoxy-1-oxomeliaca-8(30),14-dienoate (17), and methyl 3β-acetoxy-1-oxomeliaca-8(9),14-dienoate (18), were also obtained. The structures of these compounds were established on the basis of spectroscopic data or comparison with data in the literature (known compounds). The stereostructure of godavarin D was confirmed by means of single-crystal X-ray analysis. Godavarins A-C are the first mexicanolide derivatives with a C7-C28 ester-linked δ-lactone ring, while godavarins D-G are further additions to the small group of limonoids with a C1-C29 oxygen bridge. Godavarin H is a phragmalin with five acetoxy groups. Two limonoids, mexicanolide and fissinolide, were found to exhibit marked antifeedant activity against the third-instar larvae of Brontispa longissima (Gestro) at a concentration of 0.5 mg/mL. The most potent compound was mexicanolide. It also showed moderate insecticidal activity. 相似文献
4.
Pike KG Allen JV Caulkett PW Clarke DS Donald CS Fenwick ML Johnson KM Johnstone C McKerrecher D Rayner JW Walker RP Wilson I 《Bioorganic & medicinal chemistry letters》2011,21(11):3467-3470
The continued optimization of a series of glucokinase activators is described, including attempts to understand the interplay between molecular structure and the composite parameter of unbound clearance. These studies resulted in the discovery of a new scaffold for glucokinase activators and further exploration of this scaffold led to the identification of GKA60. GKA60 maintains an excellent balance of potency and physical properties whilst possessing a significantly different, but complimentary, pre-clinical pharmacokinetic profile compared with the previously disclosed compound GKA50. 相似文献
5.
Abir El Majzoub Isabelle Déchamps-Olivier Michel Aplincourt 《Inorganica chimica acta》2009,362(4):1169-4526
The Zn2+ and Cu2+ complexes of L1 and L2 ligands (L1: 1-(benzimidazol-2-ylmethyl)-1,4,7,10-tetraazacyclododecane, L2: 1,7-bis(benzimidazol-2-ylmethyl)-1,4,7,10-tetraazacyclododecane) were synthesised and characterised by means of NMR, EPR, and UV-Vis spectroscopies, X-ray determination and molecular modelisation (HF-DFT(B3LYP)/LANL2DZ). These studies showed that the 1:1 complexes were formed in which the benzimidazole arm(s) are coordinated to the metal ion. On addition of successive amounts of Zn2+ in CH3CN, the fluorescence emission of L1 increased linearly by a factor of 50 and the one of L2 by a factor of 5 while on addition of successive amounts of Cu2+ in CH3CN, the fluorescence emission of L2 decreased linearly to 80% of its initial value. 相似文献
6.
Gallant M Beaulieu C Berthelette C Colucci J Crackower MA Dalton C Denis D Ducharme Y Friesen RW Guay D Gervais FG Hamel M Houle R Krawczyk CM Kosjek B Lau S Leblanc Y Lee EE Levesque JF Mellon C Molinaro C Mullet W O'Neill GP O'Shea P Sawyer N Sillaots S Simard D Slipetz D Stocco R Sørensen D Truong VL Wong E Wu J Zaghdane H Wang Z 《Bioorganic & medicinal chemistry letters》2011,21(1):288-293
7.
High throughput screening of the Roche compound library identified benzanilides such as 1 and 2 as antagonists of TAAR1. Optimisation of this hit series led to the first selective TAAR1 antagonist (N-(3-Ethoxy-phenyl)-4-pyrrolidin-1-yl-3-trifluoromethyl-benzamide EPPTB (RO5212773, 9f) having IC50 of 28 nM at mouse TAAR1. 相似文献
8.
Chin-Pei Chang 《Inorganica chimica acta》2010,363(2):412-3748
The reaction of (η5-C5H4iPr)Co(PPh3)2 with PhCCPPh2 furnished two isomeric cyclobutadiene-substituted Cp′CoCb diphosphines, [(η5-C5H4iPr)Co(η4-1,2-(PPh2)2C4Ph2)] (5-cis) and [(η5-C5H4iPr)Co(η4-1,3-(PPh2)2C4Ph2)] (5-trans). Further reaction of 5-cis with one molar equivalent of Pd(COD)Cl2 gave palladium complex [(η5-C5H4iPr)Co(η4-1,2-(PPh2)2C4Ph2)-PdCl2] (6) in good yield. Both of the molecular structures of 5-cis and 6 were determined by single-crystal X-ray diffraction methods. Unexpectedly, the palladium complex 6 was found to be more efficient than the combination of the commonly used Buchwald’s ligand, biphenyl-2-yl-di-tert-butyl-phosphane, with Pd(OAc)2 as the catalytic precursor in the Suzuki-Miyaura reaction between ferroceneboronic acid and 4-bromoaldehyde. The X-ray structural analysis and DFT study of several palladium complexes containing sandwich-type diphosphine chelating ligands revealed that the variations in bite angles are much larger than those in bite distances. The more energetically favorable conformation in the Pd(II) complexes is the one with bite angle close to 90°. 相似文献
9.
Aurkie Ray Guillaume Pilet Carlos J. Gómez-García Sebastián Bellú 《Inorganica chimica acta》2011,375(1):20-30
A tridentate NNO donor Schiff base ligand [(1Z,3E)-3-((pyridin-2-yl)methylimino)-1-phenylbut-1-en-1-ol = LH] in presence of azide ions coordinates with cobalt(II) and copper(II) ions giving rise to three new coordination complexes [Co2(L)2(μ1,1-N3)2(N3)2] (1), [Cu2(L)2(μ1,3-N3)]·ClO4 (2) and [(μ1,1-N3)2Cu5(μ-OL)2(μ1,1-N3)4(μ1,1,1-N3)2]n (3). The complexes have been characterized by elemental analysis, FT-IR, UV-Vis spectral studies, and single crystal X-ray diffraction studies. These complexes demonstrate that under different synthetic conditions the azide ions and the Schiff base ligand (LH) show different coordination modes with cobalt(II) and copper(II) ions, giving rise to unusual dinuclear and polynuclear species (1, 2 and 3) whose structural variations are discussed. Magneto-structural correlation for the very rare singly μ1,3-N3 bridged CuII-Schiff base dinuclear species (2) has been studied. In addition, the catalytic properties of 1 for alkene oxidation and the general catalase-like activity behavior of 2 have been discussed. 相似文献
10.
Linda Näsvik Öjemyr Amandine Maréchal Henrik Vestin Brigitte Meunier Peter R. Rich Peter Brzezinski 《BBA》2014
We have studied internal electron transfer during the reaction of Saccharomyces cerevisiae mitochondrial cytochrome c oxidase with dioxygen. Similar absorbance changes were observed with this yeast oxidase as with the previously studied Rhodobacter sphaeroides and bovine mitochondrial oxidases, which suggests that the reaction proceeds along the same trajectory. However, notable differences were observed in rates and electron-transfer equilibrium constants of specific reaction steps, for example the ferryl (F) to oxidized (O) reaction was faster with the yeast (0.4 ms) than with the bovine oxidase (~ 1 ms) and a larger fraction CuA was oxidized with the yeast than with the bovine oxidase in the peroxy (PR) to F reaction. Furthermore, upon replacement of Glu243, located at the end of the so-called D proton pathway, by Asp the PR → F and F → O reactions were slowed by factors of ~ 3 and ~ 10, respectively, and electron transfer from CuA to heme a during the PR → F reaction was not observed. These data indicate that during reduction of dioxygen protons are transferred through the D pathway, via Glu243, to the catalytic site in the yeast mitochondrial oxidase. This article is part of a Special Issue entitled: 18th European Bioenergetic Conference. 相似文献
11.
Two oxime-functionalized diazamesocyclic derivates, namely, N,N′-bis(acetophenoneoxime)-1,4-diazacycloheptane (H2L1) and N,N′-bis(acetophenonoxime)-1,5-diazacyclooctane (H2L2), have been prepared and characterized. Both ligands (obtained in the hydrochloride form) can form stable metal complexes with CuII and NiII salts, the crystal structures of which were determined by X-ray diffraction technique. The reactions of H2L1 with Cu(ClO4)2 and Ni(ClO4)2 afford a penta-coordinated mononuclear complex [Cu(H2L1)Cl] · ClO4 (1) and a four-coordinated monomeric [Ni(HL1)] · ClO4 (2), in which the ligand is monodeprotonated. The ligand H2L2 also forms a quite similar mononuclear [Ni(HL2)] · ClO4 complex with Ni(ClO4)2, according to our previous work. However, reactions of different CuII salts [Cu(ClO4)2, CuCl2 and Cu(NO3)2 for 3, and CuSO4 for 4] with H2L2 in the presence of NaClO4 yield two unusual mono-μ-Cl dinuclear CuII complexes [Cu2(HL2)2Cl] · (ClO4) (3), and [Cu2(H2L2)(HL2)Cl] · (ClO4)2 · (H2O)(4). These results indicate that the resultant CuII complexes (1, 3 and 4) are sensitive to the backbones of diazamesocycles and even auxiliary anions. 相似文献
12.
Bernadette S. Creaven Timothy McCormac Ann-Marie Moore 《Inorganica chimica acta》2005,358(9):2661-2670
Two functionalised calix[4]arenes, 5,11,17,23-tetra-tert-butyl-25,27-bis(2-pyridylmethoxy)calix[4]arene (L1) and 5,11,17,23-tetra-tert-butyl-25,27-bis(2-pyridylmethoxy)-26,28-dibutoxycalix[4]arene (L3), were prepared and characterised. The copper(I) complexes of both calix[4]arenes were synthesised and their reactivities were analysed and compared. The presence of the metal induced a radical in the case of L1 whereas no such radical was observed in the metal complex of ligand L3. 相似文献
13.
Fox BM Natero R Richard K Connors R Roveto PM Beckmann H Haller K Golde J Xiao SH Kayser F 《Bioorganic & medicinal chemistry letters》2011,21(8):2460-2467
We discovered novel pyrrolidine MCHR1 antagonist 1 possessing moderate potency. Profiling of pyrrolidine 1 demonstrated that it was an inhibitor of the hERG channel. Investigation of the structure-activity relationship of this class of pyrrolidines allowed us to optimize the MCHR1 potency and decrease the hERG inhibition. Increasing the acidity of the amide proton by converting the benzamide in lead 1 to an anilide provided single digit nanomolar MCHR1 antagonists while replacing the dimethoxyphenyl ring of 1 with alkyl groups possessing increased polarity dramatically reduced the hERG inhibition. 相似文献
14.
So Young Lee 《Inorganica chimica acta》2009,362(4):1047-3853
Two isomeric dibenzo-O2S2 macrocycles L1 and L2 have been synthesised and their coordination chemistry towards palladium(II) has been investigated. Two-step approaches via reactions of 1:1-type complexes, [cis-Cl2LPd] (1a: L = L1, 1b: L = L2), with different O2S2 macrocycle systems (L1 and L2) have led to the isolation of the following bis(O2S2 macrocycle) palladium(II) complexes in the solid state: [Pd(L1)2](ClO4)2 (2a) and a mixture of [Pd(L1)2](ClO4)2 (2a) + [Pd(L2)2](ClO4)2 (2b). 相似文献
15.
Jun-Jie Wang 《Inorganica chimica acta》2010,363(7):1377-1385
In our continuing efforts to explore the effects of substituent groups of ligands in the formation of supramolecular coordination structures, seven new CuII complexes formulated as [Cu2(L1)4(DMF)2] (1), {[Cu2(L1)4(Hmta)](H2O)0.75}∞ (2), [Cu2(L2)4(2,2′-bipy)2] (3), [Cu2(L3)4(H2O)2] (4), [Cu2(L3)4(Hmta)]∞ (5), [Cu2(L3)4(Dabco)]∞ (6) and [Cu2(L3)4(Pz)]∞ (7) with three monocarboxylate ligands bearing different substituent groups HL1-HL3 (HL1 = phenanthrene-9-carboxylic acid, HL2 = 2-phenylquinoline-4-carboxylic acid, HL3 = adamantane-1-carboxylic acid, Hmta = hexamethylenetetramine, 2,2′-bipy = 2,2′-bipyridine, Dabco = 1,4-diazabicyclo[2.2.2] octane and Pz = pyrazine), have been prepared and characterized by X-ray diffraction. In 1, 2 and 4-7, each CuII ion is octahedrally coordinated, and carboxylate acid acts as a syn-syn bridging bidentate ligand. While each CuII ion in 3 is penta-coordinated in a distorted square-pyramidal geometry. 1 and 4 both show a dinuclear paddle-wheel block, while 2, 5, 6 and 7 all exhibit an alternated 1D chain structure between dinuclear paddle-wheel units of the tetracarboxylate type Cu2-(RCO2)4 and the bridging auxiliary ligands Hmta, Dabco and Pz. Furthermore, 3 has a carboxylic unidentate and μ1,1-oxo bridging dinuclear structure with the chelating auxiliary ligand 2,2′-bipy. Moreover, complexes 1-6 were characterized by electron paramagnetic resonance (EPR) spectroscopy. 相似文献
16.
Subash Chandra Sahoo 《Inorganica chimica acta》2010,363(12):3055-373
Four different mononuclear octahedral Ni(II) complexes with protonated and deprotonated form of the same ligand have been synthesized by controlling reaction conditions and structurally characterized. The complexes are [Ni(HLl-his)(benzoate)(MeOH)] (1), [Ni(HLl-his)(SCN)(MeOH)] (2), [Ni(HLl-his)2] (3) and [Ni(Ll-his)(imidazole)2] (4) where H2Ll-his is (S)-2-(2-hydroxybenzylamino)-3-(1H-imidazol-4-yl)-propionic acid. The ligand behaves as a monobasic tetradentate ligand in 1 and 2, monobasic tridentate ligand in 3 and dibasic tetradentate ligand in 4. Ni(II) coordinated phenolic proton of the ligand in the complexes 1-2 shows strong intra-molecular H-bonding with benzoate in 1 and lattice water in 2, whereas 3 shows intermolecular H-bonding between uncoordinated phenols with neighbouring carboxylate. The pH titration of the complexes revealed that metal coordination and H-bond in complexes 1 and 2 considerably lowers the acidity of ligand phenol (pKa 6.8 and 7.0 respectively) compared to phenol (pKa 10). The complex 4 does not show any proton loss due to the absence of phenolic proton. All the complexes show extensive H-bonded network in the crystals including narrow (7.8 × 5.2 Å) water filled one dimensional channel in 2. 相似文献
17.
New hydrogen-bonding assemblies were synthesized from the reaction of a metalloligand, [Cu(2,4-pydca)2]2− (LCu) (2,4-pydca = 2,4-pyridinedicarboxylate), with a FeII ion or an imidazole in an aqueous medium and crystallographically characterized. The obtained compounds, [Fe(H2O)6][Cu(2,4-pydca)2] (1) and [Cu(2,4-pydca)(imidazole)2] · 2H2O (2), have metalloligand dimer units, [Cu2(2,4-pydca)4]4− and [Cu2(2,4-pydca)2(imidazole)4], respectively, each of which assembles by π-π (1) and hydrogen-bonding (2) interactions to form 1-D metalloligand arrays. The 1-D metalloligand arrays are linked by rich hydrogen-bonding interactions via H2O molecules. 相似文献
18.
Ryszard Kubiak 《Inorganica chimica acta》2010,363(11):2461-2466
Two crystals of holmium(III) double-decker iodine doped phthalocyanines, HoPc2I5/3 (I) and HoPc2I (II), were grown directly in the reaction of holmium chips with 1,2-dicyanobenzene under versatile quantity of iodine at 180-160 °C. The complex I crystallises in the P4/mcc space group of tetragonal system, while the complex II crystallises in the P2/c space group of monoclinic system. The space group of P4/mcc and z = 1 requires that the Ho(III) atom is statistically disordered in the HoPc2I5/3 structure. The iodine atoms form linear symmetrical triiodide ions in I, while the I− ions in II. Assignment of iodine species as in the HoPc2I5/3 and I− in HoPc2I complexes point to the +5/9 and +1 oxidation state of the HoPc2 unit in these complexes. Thus one Pc macrocycle of the double-decker HoPc2 units has a non-integer oxidation state of −1.222 in I, while both Pc-rings are one-electron oxidised radical Pc− in II. Magnetic susceptibilities of HoPc2I5/3 and HoPcI at room temperature are 4.56 × 10−2 and 5.12 × 10−2 emu/mol and the calculated magnetic moments are 10.46 and 11.08 μB, respectively. UV-Vis spectroscopic measurement of I and II in benzene solution were carried out and discussed. 相似文献
19.
Zdeněk Trávní?ek Igor Popa Radek Zbo?il Ji?í Mikulík 《Journal of inorganic biochemistry》2010,104(4):405-11728
The first FeIII complexes 1-6 with cyclin-dependent kinase (CDK) inhibitors of the type [Fe(Ln)Cl3]·nH2O (n = 0 for 1, 1 for 2, 2 for 3-6; L1-L6 = C2- and phenyl-substituted CDK inhibitors derived from 6-benzylamino-9-isopropylpurine), have been synthesized and characterized by elemental analysis, IR, 57Fe Mössbauer, 1H and 13C NMR, and ES+ mass spectroscopies, conductivity and magnetic susceptibility measurements, and thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). The study revealed that the compounds are mononuclear, tetrahedral high-spin (S = 5/2) FeIII complexes with an admixture of an S = 3/2 spin state originating probably from five-coordinated FeIII ions either connecting with a bidentate coordination mode of the CDK inhibitor ligand or relating to the possibility that one crystal water molecule enters the coordination sphere of the central atom in a portion of molecules of the appropriate complex. Nearly spin-only value of the effective magnetic moment (5.82 μeff/μB) was determined for compound 1 due to absence of crystal water molecule(s) in the structure of the complex. Based on NMR data and DFT calculations, we assume that the appropriate organic ligand is coordinated to the FeIII ion through the N7 atom of a purine moiety. The cytotoxicity of the complexes was tested in vitro against selected human cancer cell lines (G-361, HOS, K-562 and MCF-7) along with the ability to inhibit the CDK2/cyclinE kinase. The best cytotoxicity (IC50: 4-23 μM) and inhibition activity (IC50: 0.02-0.09 μM) results have been achieved in the case of complexes 2-4, and complexes 3, 4 and 6, respectively. In addition, the X-ray structure of 2-chloro-6-benzylamino-9-isopropylpurine, i.e. a precursor for the preparation of L1, L4 and L5, is also described. 相似文献
20.
The acid-base properties and Cu(II), Ni(II), Ag(I) and Hg(II) binding abilities of PAMAM dendrimer, L, and of the simple model compounds, the tetraamides of EDTA and PDTA, L1, were studied in solution by pH-metric methods and by 1H NMR and UV-Vis spectroscopy. PAMAM is hexabasic and six pKa values have been determined and assigned. PAMAM forms five identifiable complexes with copper(II), [CuLH4]6+, [CuLH2]4+, [CuLH]3+, [CuL]2+ and [CuLH-1]+ in the pH range 2-11 and three with nickel(II), [NiLH]3+, [NiL]2+ and [NiLH-1]+ in the pH range 7-11. The complex [CuLH4]6+, which contains two tertiary nitrogen and three amide oxygen atoms coordinated to the metal ion, is less stable than the analogous EDTA and PDTA tetraamide complexes [CuL1]2+, which contain two tertiary nitrogen and four amide oxygen atoms, due to ring size and charge effects. With increasing pH, [CuLH4]6+ undergoes deprotonation of two coordinated amide groups to give [CuLH2]4+ with a concomitant change from O-amide to N-amidate coordination. Surprisingly and in contrast to the tetraamide complexes [CuL1]2+, these two deprotonation steps could not be separated. As expected the nickel(II) complexes are less stable than their copper(II) analogues. The tetra-N-methylamides of EDTA, L1(b), and PDTA form mononuclear and binuclear complexes with Hg(II). In the case of L1(b) these have stoichiometries HgL1(b)Cl2, [HgL1(b)H−2Cl2]2−, [Hg2L1(b)Cl2]2+, Hg2L1(b)H−2Cl2 and [Hg2L1(b)H−5Cl2]3−. Based on 1H NMR and pH-metric data the proposed structure for HgL1(b)Cl2, the main tetraamide ligand containing species in the pH range <3-6.5, contains L1(b) coordinated to the metal ion through the two tertiary nitrogens and two amide oxygens while the structure of [HgL1(b)H−2Cl2]2−, the main tetraamide ligand species at pH 7.5-9.0, contains the ligand similarly coordinated but through two amidate nitrogen atoms instead of amide oxygens. The proposed structure of [Hg2L1(b)Cl2]2+, a minor species at pH 3-6.5, also based on 1H NMR and pH-metric data, contains each Hg(II) coordinated to a tertiary amino nitrogen, two amide oxygens and a chloride ligand while that of [Hg2L1(b)H−5Cl2]3−, contains each Hg(II) coordinated to a tertiary amino nitrogen, two amidate nitrogens, a chloride and a hydroxo ligand in the case of one of the Hg(II) ions. The parent EDTA and PDTA amides only form mononuclear complexes. PAMAM also forms dinuclear as well as mononuclear complexes with mercury(II) and silver(I). In the pH range 3-11 six complexes with Hg(II) i.e. [HgLH4Cl2]4+, [HgLH3Cl2]3+, [Hg2LCl2]2+, [Hg2LH−1Cl2]+, [HgLH−1Cl2]− and [HgLH−2Cl2]2− were identified and only two with Ag(I), [AgLH3]4+ and [Ag2L]2+. Based on stoichiometries, stability constant comparisons and 1H NMR data, structures are proposed for these species. Hence [HgLH4Cl2]4+ is proposed to have a similar structure to [CuLH4]6+ while [Hg2LCl2]2+has a similar structure to [Hg2L1(b)H−5Cl2]3−. 相似文献