共查询到20条相似文献,搜索用时 15 毫秒
1.
Joana T. Zaharieva Maria Milanova Dimitar Todorovsky 《Central European Journal of Chemistry》2012,10(6):1907-1912
The paper considers the possibilities for mechanochemical synthesis of rare earth complexes. The complex Eu(TTA)3·phen (HTTA — 2-thenoyltrifluoroacetone, phen — 1,10-phenanthroline) is synthesized by mechanical treatment of a mixture of EuCl3.6H2O, HTTA, phen and NaOH in planetary ball mill Pulverisette 7 for 30 min at 800 min?1. The non reacted starting reagents and reaction side products are separated by treating activated mixture with water-ethanol solution following a procedure proposed in the literature. The elemental composition, X-ray diffraction pattern, IR spectra, optical properties (excitation and emission spectra, luminescence lifetime) and morphology of the mechanochemically synthesized complex are compared with those of the complex prepared from solution by the conventional method. The results confirm close similarity in the molecular structure and identity of the elemental composition, X-ray diffractograms and fluorescence properties of the compounds prepared by both methods. 相似文献
2.
3.
Hsien-Chang Kao 《Tetrahedron letters》2010,51(29):3743-3747
A family of acyclic aza-bridged bis-1,10-phenanthroline compounds has been synthesized in a convenient way. The resulting compounds 2 and 2·HCl were fully characterized and their solid state structures and NMR spectroscopic properties were investigated to assess how the structural units affect the alkylation reactions. The results reveal the transoid structure for 2. The broadening NMR peak in 2 is shown to be due to an unusual intramolecular CH?N hydrogen bond. This unique conformation offers an efficient and regioselective method to prepare the amino-substituted bis-2,2′-1,10-phenanthroline derivatives and 1,10-phenanthrolino-N-alkylated compounds. 相似文献
4.
5.
A. Moodi M. Khorasani-Motlagh M. Noroozifar B. O. Patrick 《Journal of Structural Chemistry》2014,55(2):337-341
YCl3·6H2O reacts with 1,10-phenanthroline (phen) to yield a complex of 1:2 yttrium:ligand stoichiometry. The yttrium(III) complex is characterized by the elemental analysis, UV-Vis, IR as well as the X-ray diffraction analysis. The crystal of [Y(phen)2Cl(H2O)3]Cl2·H2O obtained from a methanol solution crystallizes in the triclinic system, space group P 337-1, Z = 2, a = 10.3236(4) Å, b = 10.4566(4) Å, c = 12.5270(5) Å, α = 97.354(2)°, β = 108.740(2)°, γ = 93.458(2)°, R int = 0.046. The Y(III) ion is eight-coordinated by four nitrogen, three oxygen atoms and one chlorine atom. 相似文献
6.
A new mixed-ligand V(IV) complex, [VO(o-Van-Val)(phen)]·CH3CN (o-Van-val = Schiff base derived from o-vanillin and l-valine, phen = 1,10-phenanthroline), was synthesized and characterized by physico-chemical methods and single-crystal X-ray diffraction. In the crystal, the V(IV) atom is six-coordinated by one oxo ligand, two oxygen atoms and one nitrogen atom from a valine Schiff base ligand, and two nitrogen atoms from 1,10-phenanthroline, giving a distorted octahedral arrangement. The DNA-binding properties of the complex were investigated by spectroscopic methods and viscosity measurements. The results suggest that the oxovanadium(IV) complex binds to DNA in an intercalation mode. 相似文献
7.
《Journal of Coordination Chemistry》2012,65(3):400-409
Two d10 group 12 metal complexes, 2-(2-methoxyphenyl)-1,10-phenanthroline zinc dichloride (2a) and 2-(2-methoxyphenyl)-1,10-phenanthroline mercury dichloride (2b) were synthesized and characterized by IR, 1H and 13C NMR as well as elemental analysis. Structure of 2b in the solid state was determined by single-crystal X-ray crystallography, revealing that 2b is four-coordinate in a distorted tetrahedral geometry with the methoxy group uncoordinated. Luminescent properties of 2a and 2b in solution and the solid state were studied. 相似文献
8.
《Journal of Coordination Chemistry》2012,65(17):1473-1480
A new copper complex, [Cu(phen)2N3]ClO4 (phen = 1,10-phenanthroline), has been synthesized and characterized by X-ray single-crystal structure analysis. The copper atom is five-coordinated with four nitrogen atoms of two phens and one nitrogen atom of the azide to form an intermediate coordination geometry distorted from trigonal bipyramidal (TBP) and square pyramidal (SP). The extended three-dimensional structure is formed through π–π interactions and hydrogen bonds. The IR spectrum, electronic spectrum, magnetic properties and ESR spectrum of the title compound have been studied. 相似文献
9.
A binuclear terbium complex with 2,4,6-Trimethylbenzoate and 1,10-phenanthroline, [Tb2(TMBA)6(Phen)2], has been synthesized (TMBA=2,4,6-Trimethylbenzoic acid and phen=1,10-phenanthroline) and characterized by IR, elemental analysis and X-ray diffraction methods. The title complex crystallizes in monoclinic system, space group P21/c with a=1.327 5(2) nm, b=2.817 9(5) nm, c=1.282 5(2) nm, β=116.692(3)°, V=4.286 2(13) nm3, Z=4,Dc=1.423 g·cm-3. There are four bridged carboxylate groups of the 2,4,6-trimethylbenzoic acid bonded to the two terbium ions, each ions is also chelated with the two oxygen atoms of a molecule of the 2,4,6-trimethylbenzoic acid and the two nitrogen atoms of a 1,10-phenanthroline respectively, forming a 8-coordination distorted square antiprism. Average Tb-O and Tb-Ndistance of the two Tb(Ⅲ) ions are equal respectively. This shows the two terbium ions are in the same chemical enviorments. The complex emits intense green fluorescence under ultraviolet light. CCDC: 619215. 相似文献
10.
《Journal of Coordination Chemistry》2012,65(2):273-283
The saccharinato complexes [Zn(phen)2(sac)(H2O)]sac (1) and [Zn(sac)(dmp)(H2O)](sac) (2), where phen = 1,10-phenanthroline, dmp = 2,9-dimethyl-1,10-phenanthroline, and sac =saccharinato ion/ligand, were synthesized by the reaction of [Zn(sac)2(H2O)4] · 2H2O with ligands and have been characterized by elemental analysis, IR, and 1H NMR spectroscopies. Conductivity of complexes was measured in DMSO. Compound 1 is characterized by single crystal X-ray diffraction and compared with some isomorphous zinc-saccharinate complexes reported previously. Complex 1 crystallizes in the triclinic system, space group P 1 , with Z = 2, and consists of alternating slightly distorted octahedral [Zn(phen)2(sac)(H2O)]+ and noncoordinated saccharinate. The zinc bound aqua is hydrogen bonded to an oxygen of carbonyl in the saccharinate ligand and the SO2 group in the saccharinate counter-ion from an adjacent molecule. Intermolecular and intramolecular hydrogen bonds and C–H ··· O and C–H ··· N short contacts lead to a 3-D network. 相似文献
11.
I. V. Kalinovskaya I. A. Tkachenko A. G. Mirochnik V. E. Karasev V. Ya. Kavun 《Russian Journal of General Chemistry》2012,82(4):676-678
Luminescent and magnetic properties of the europium nitrate complex with 1,10-phenanthroline synthesized in the traditional way by precipitation from water-ethanol medium and by the method of mechanical activation were investigated. Correlations between luminescent and magnetic properties of the complex compounds were revealed. The higher value of molar magnetic susceptibility ??m was shown to be typical for the highly dispersed europium compound obtained by mechanochemistry method due to the presence of the paramagnetic ion Eu2+. 相似文献
12.
A. S. Alikhanyan I. A. Solonina M. N. Rodnikova 《Russian Journal of Inorganic Chemistry》2007,52(8):1220-1222
The thermodynamic stability of neodymium nitrate complex with 1,10-phenanthroline (Phen) was determined by mass spectrometry. The complex was formulated as Nd(NO3)3 · 2C12H8N2 on the basis of elemental analysis. Mass spectrometry allowed us to characterize the decomposition of Nd(NO3)3 · 2C12H8N2 thermodynamically. The formation enthalpy of this complex is ?1058.0 kJ/mol. 相似文献
13.
《Acta Crystallographica. Section C, Structural Chemistry》2017,73(5):393-398
Binuclear and tetranuclear copper(II) complexes are of interest because of their structural, magnetic and photoluminescence properties. Of the several important configurations of tetranuclear copper(II) complexes, there are limited reports on the crystal structures and solid‐state photoluminescence properties of `stepped' tetranuclear copper(II) complexes. A new CuII complex, namely bis{μ3‐3‐[(4‐methoxy‐2‐oxidobenzylidene)amino]propanolato}bis{μ2‐3‐[(4‐methoxy‐2‐oxidobenzylidene)amino]propanolato}tetracopper(II), [Cu4(C11H13NO3)4], has been synthesized and characterized using elemental analysis, FT–IR, solid‐state UV–Vis spectroscopy and single‐crystal X‐ray diffraction. The crystal structure determination shows that the complex is a stepped tetranuclear structure consisting of two dinuclear [Cu2(L )2] units {L is 3‐[(4‐methoxy‐2‐oxidobenzylidene)amino]propanolate}. The two terminal CuII atoms are four‐coordinated in square‐planar environments, while the two central CuII atoms are five‐coordinated in square‐pyramidal environments. The solid‐state photoluminescence properties of both the complex and 3‐[(2‐hydroxy‐4‐methoxybenzylidene)amino]propanol (H2L ) have been investigated at room temperature in the visible region. When the complex and H2L are excited under UV light at 349 nm, the complex displays a strong blue emission at 469 nm and H2L displays a green emission at 515 nm. 相似文献
14.
Zheng SL Gembicky M Messerschmidt M Dominiak PM Coppens P 《Inorganic chemistry》2006,45(23):9281-9289
By selection of different charge-balancing anionic frameworks and different host-to-guest ratios, the photosensitizer-dye cation [Cu(dmp)2]+ (dmp = 2,9-dimethyl-1,10-phenanthroline) has been embedded in a series of three-dimensional host structures. It occurs with variable geometry in different states of aggregation, including weakly interacting monomers, isolated dimers, columns, and layers. A large variation in its emission lifetime is correlated with the relative energy level spacings of the guest- and host-framework components. In a fully saturated host framework, the lifetime exceeds values reported for a series of conventional Cu(dmp)2 salts. 相似文献
15.
《Journal of Coordination Chemistry》2012,65(15):2488-2498
A ternary copper(II) complex, [Cu(phen)(L-Gly)(H2O)] ·?NO3 ·?1.5H2O (phen =?1,10-phenanthroline, L-Gly =?L-glycine), has been synthesized and structurally characterized. The complex crystallized in a monoclinic system with space group C2/c, a =?20.572(3) Å, b =?6.9987(10) Å, c =?23.561(3) Å, β?= 98.776(5)°. The five-coordinate copper(II) center is a distorted square pyramid. Absorption spectra, fluorescence spectra and viscosity measurements showed interaction between the copper complex and DNA through an intercalative mode. The complex exhibited efficient DNA cleavage activity at micromolar concentration in the presence of ascorbate with hydroxyl radicals as the active species. 相似文献
16.
I. V. Kalinovskaya V. G. Kuryavyi P. P. Safronov V. E. Karasev 《Russian Journal of Physical Chemistry A, Focus on Chemistry》2008,82(13):2173-2175
Mechanochemically synthesized europium nitrate with 1,10-phenanthroline (Phen) is formed into globules with sizes of 100–300
nm, which are assembled into larger globular aggregates or packed into layers. The increasing mechanical activation time induces
sintering, generating porous aggregates with micro-and nanopores. Eu2+ paramagnetic centers, detectable by ESR, are generated by mechanical grinding. Possibly, they are positioned on the surfaces
of nanoglobules. The complex Eu(NO3)3 · 2Phen synthesized conventionally from aqueous ethanol consists of needle-shaped microcrystallites. They do not give rise
to ESR spectra. 相似文献
17.
A. Paul Krapcho Silvia Sparapani Amber Leenstra Joshua D. Seitz 《Tetrahedron letters》2009,50(26):3195-3747
The synthesis and structural assignments of 9-chloro-1,1-phenanthroline-2(1H)-thione and 1,10-dihydro-1,10-phenanthroline-2,9-dithione have been accomplished. The sulfur-bridged bis-1,10-phenanthroline macrocycle was readily prepared by heating the thione or equimolar amounts of the dithione and 2,9-dichloro-1,10-phenanthroline in diphenyl ether. Displacements of 2-chloro- or 2,9-dichloro-1,10-phenanthroline with N,N-dimethylethylenediamine afforded the corresponding amine and diamino analogues. An amino-substituted-2,2′-bis-1,10-phenanthroline has been prepared. 相似文献
18.
《Journal of Coordination Chemistry》2012,65(16):1873-1882
Two lanthanide complexes with 2-fluorobenzoate (2-FBA) and 1,10-phenanthroline (phen) were synthesized and characterized by X-ray diffraction. The structure of each complex contains two non-equivalent binuclear molecules, [Ln(2-FBA)3?·?phen?·?CH3CH2OH]2 and [Ln(2-FBA)3?·?phen]2 (Ln?=?Eu (1) and Sm (2)). In [Ln(2-FBA)3?·?phen?·?CH3CH2OH]2, the Ln3+ is surrounded by eight atoms, five O atoms from five 2-FBA groups, one O atom from ethanol and two N atoms from phen ligand; 2-FBA groups coordinate Ln3+ with monodentate and bridging coordination modes. The polyhedron around Ln3+ is a distorted square-antiprism. In [Ln(2-FBA)3?·?phen]2, the Ln3+ is coordinated by nine atoms, seven O atoms from five 2-FBA groups and two N atoms of phen ligand; 2-FBA groups coordinate Ln3+ ion with chelating, bridging and chelating-bridging three coordination modes. The polyhedron around Ln3+ ion is a distorted, monocapped square-antiprism. The europium complex exhibits strong red fluorescence from 5D0?→?7F j ( j?=?1–4) transition emission of Eu3+. 相似文献
19.
The structure of tetraaqua-bis(nitrato-O,O′)-(1,10-phenanthroline-N,N′)-lanthanum(III) 1,3,5,7-tetraazatricyclo[3.3.1.13,7]decane nitrate dihydrate, [La(NO3)2 · phen · (H2O)4]+ · hmt · NO
3
−
· 2H2O, is presented. The lanthanum ion exhibits tenfold coordination and the polyhedron can be described as tetradecahedron. The
complex cations, nitrate ions, water and hexamethylenetetramine molecules are assembled via hydrogen bonds, H–π rings and π–π stacking interactions into 3D supramolecular network. The bond strength of coordination sphere was calculated by means of
the bond-valence method. The influence of La:phen stoichiometry and additional ligand on the changes of lanthanum(III) coordination
sphere geometry in ten-coordinated complexes with 1,10-phenanthroline was discussed. The infrared spectrum of structure optimised
by means of quantum mechanical calculations was analysed and compared with measured one. The obtained compound was characterised
by thermogravimetric analysis in conjunction with evolved gases in the air atmosphere. 相似文献
20.
Vahid Amani Nasser Safari Behrouz Notash 《Journal of the Iranian Chemical Society》2013,10(4):751-761
[Fe(Me-phen)Cl4][Me-phen·H] (1) and [Fe(Cl-phen)Cl4][Cl-phen·H] (2) complexes were prepared from the reactions of FeCl3·6H2O with 5-methyl-1,10-phenanthroline (Me-phen) and 5-chloro-1,10-phenanthroline (Cl-phen), respectively, in a 0.1 M aqueous solution of HCl. Stepwise addition of dimethyl sulfoxide to the solution of 1 in methanol results in a mixed ligand complex, [Fe(Me-phen)Cl3(DMSO)] (3). Complex 3 was also prepared by two other methods. The reaction of a methanol solution of [Fe(Me-phen)Cl4][Me-phen·H] (1) with [Fe(DMSO)4Cl2][FeCl4] in 1:6 ratio led to 3. Complex 3 was also prepared from the reaction of 5-methyl-1,10-phenanthroline with [Fe(DMSO)4Cl2][FeCl4] in 1:1 ratio in methanol. The three complexes were characterized by IR, UV–Vis, 1H NMR and luminescence spectroscopy and their structures were studied by the single-crystal diffraction method. Calculation methods were employed to study the isomerization of (3) in solution. 相似文献