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1.
Yu Ding Feng Wang Zong-Jun Ku Lian-Sheng Wang Huan-Bo Zhou 《Journal of Structural Chemistry》2009,50(6):1212-1215
The title compound, [Zn(pytpy)2][NO3]2·2H2O (pytpy = 4′-(4-pyridyl)-2,2′: 6′,2″-terpyridine), has been synthesized by the reaction of Zn(NO3)2·6H2O with pytpy, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to tetragonal
space group P43 with a = 0.90873(8) nm, b = 0.90873(8) nm, c = 4.4741(6) nm, V = 3.6946(7) nm3, Z = 4, D
c
= 1.521 g/cm−3, μ = 0.736 mm−1, F(000) = 1744, R = 0.0871, wR = 0.1302 for 5553 observed reflections with I > 2σ(I). X-ray analysis has revealed that the ZnII ion is surrounded by six N atoms from two pytpy ligands leading to a distorted octahedral geometry. In the crystal structure
there are numerous strong intermolecular and intramolecular H-bonds and π-π interactions. 相似文献
2.
L. A. Glinskaya V. G. Shchukin R. F. Klevtsova A. P. Mazhara S. V. Larionov 《Journal of Structural Chemistry》2001,41(4):632-639
A new mixed-ligand complex, Zn(4,4′-bipy){(i-PrO)2PS2}2, was synthesized. Single crystals were grown,and the structure of the complex was determined by X-ray diffraction (CAD-4 diffractometer, MoKα radiation, 14807 Fhkl, R =0.0391. The crystals are monoclinic with unit cell dimensions a-17.569(2), b = 26.253(5), c = 27.915(3) ?, ? =100.70(1)°, V = 12652(3) ?3, Z = 16, dvalc = 1.361 g/cm3, space group P21/n. The structure is formed from infinite zigzag polymer chains stretched along the a axis. The coordination polyhedron of
the Zn atom is a distorted tetrahedron formed by two S atoms of two monodentate diisopropyldithiophosphate ligands and two
N atoms of two bridging bidentate 4,4′-bipy molecules. When heated in vacuum, the compounds ZnL{(i-PrO)2PS2}2 (L) =phen, 2,2′-bipy, 4,4′-bipy are volatile.
Translated fromZhurnal Strukturnoi Khimii, Vol. 41, No. 4, pp. 772-780, July-August, 2000 相似文献
3.
D. Czakis-Sulikowska A. Czylkowska J. Radwańska-Doczekalska R. Grodzki E. Wojciechowska 《Journal of Thermal Analysis and Calorimetry》2007,90(2):557-564
New mixed-ligands complexes with empirical formulae: M(2,4′-bpy)2L2·H2O (M(II)Zn, Cd), Zn(2-bpy)3L2·4H2O, Cd(2-bpy)2L2·3H2O, M(phen)L2·2H2O (where M(II)=Mn, Ni, Zn, Cd; 2,4′-bpy=2,4′-bipyridine, 2-bpy=2,2′-bipyridine, phen=1,10-phenanthroline, L=HCOO−) were prepared in pure solid state. They were characterized by chemical, thermal and X-ray powder diffraction analysis, IR
spectroscopy, molar conductance in MeOH, DMF and DMSO. Examinations of OCO− absorption bands suggest versatile coordination behaviour of obtained complexes. The 2,4′-bpy acts as monodentate ligand; 2-bpy and phen as chelating ligands. Thermal studies were performed in static air atmosphere. When the temperature raised the dehydration
processes started. The final decomposition products, namely MO (Ni, Zn, Cd) and Mn3O4, were identified by X-ray diffraction. 相似文献
4.
Yan Ding Hongli Chen Weilin Chen Enbo Wang Jingxin Meng 《Transition Metal Chemistry》2009,34(3):281-288
Four novel organic–inorganic hybrid compounds [Cu5
I(4,4′-bpy)3(2,2′-bpy)4][BW12O40] · H2O (1), [Ni0.5(2,2′-bpy)1.25][Ni(2,2′-bpy)3][Ni(2,2′-bpy)2(H2O)(SiW11VIWVO40)] · 0.5H2O (2), [H2bpy]2[Zn(2,2′-bpy)3]2[Si2W18O62] · 1.5H2O (3) and [CuII(2,2′-bpy)2]2[SiW12O40] · 2H2O (4) (2,2′-bpy = 2,2′-bipyridine, 4,4′-bpy = 4,4′-bipyridine) have been synthesized under hydrothermal conditions and characterized
by elemental analysis, IR spectroscopy, thermal gravimetric analysis, electrochemical measurements and single-crystal X-ray
diffraction. Compound (1) is a novel [BW12O40]5− polyoxoanion bisupported by copper(I) coordination cations with mixed 2,2′-bpy and 4,4′-bpy ligands. Compound (2) is constructed from the [SiW11VIWVO40]5− polyoxoanions supported by [Ni(2,2′–bpy)2]2+. Compound (3) is composed of a novel [Si2W18O62]8− cluster and [Zn(2,2′–bpy)3]2+ complexes, which held together into a three-dimensional (3D) supramolecular network through hydrogen-bonding interactions.
Compound (4) shows a 2D layer framework constructed from a bisupporting Keggin polyoxoanion cluster and [Cu(2,2′–bpy)2]2+ coordination polymer fragments, resulting in 3D networks via supramolecular interactions.
Electronic supplementary material The online version of this article (doi:) contains supplementary material, which is available to authorized users. 相似文献
5.
N. M. Kurochkina V. E. Baulin E. N. Pyatova I. S. Ivanova A. Yu. Tsivadze 《Russian Journal of Coordination Chemistry》2010,36(4):241-248
Sodium and potassium complexes with 4′-(4‴-benzo-15-crown-5)methyloxy-2,2′:6′,2″-terpyridine (L1) and 4′-(4′-benzo-15-crown-5)oxy-2,2′:6′,2″-terpyridine (L2) and heteronuclear Na, K, Ca, and transition metal complexes with L1 were synthesized. The structure of the complexes was proposed on the basis of elemental analysis data, IR spectra, and the
results of earlier X-ray diffraction studies of L2, [NaL1NCS], and [Na2{Cu(L1)2}(NCS)3]NCS · CH3CN. 相似文献
6.
M. Aksu S. Durmu M. Sari K. C. Emregül I. Svoboda H. Fuess O. Atakol 《Journal of Thermal Analysis and Calorimetry》2007,90(2):541-547
N,N′-bis(salicylidene)-1,3-propanediamine (LH2), N,N′-bis(salicylidene)-2,2′-dimethyl-1,3-propanediamine (LDMH2), N,N′-bis(salicylidene)-2-hydroxy-1,3-propanediamine (LOH3), N,N′-bis(2-hydroxyacetophenylidene)-1,3-propanediamine (LACH2) and N,N′-bis(2-hydroxyacetophenone)-2,2′-dimethyl-1,3-propanediamine (LACDMH2) were synthesized and reduced to their phenol-amine form in alcoholic media using NaBH4 (LHH2, LDMHH2, LOHHH2, LACHH2 and LACDMHH2). Heterodinuclear complexes were synthesized using Ni(II), Zn(II) and Cd(II) salts, according to the template method in DMF
media.
The complex structures were analyzed using elemental analysis, IR spectroscopy, and thermogravimetry. Suitable crystals of
only one complex were obtained and its structure determined using X-ray diffraction, NiLACH·CdBr2·DMF2, space group orthorhombic, Pbca, a=20.249, b=14.881, c=20.565 ? and Z=8. The heterodinuclear complexes were seen to be of [Ni·ligand·MX2·DMF2] structure (ligand=LH2−, LDMH2−, LOHH2−, LACH2−, LACDMH2−, M=ZnII, CdII, X=Br−, I−). Thermogravimetric analysis showed irreversible bond breakage of the coordinatively bonded DMF molecules followed by decomposition
at this temperature. 相似文献
7.
Three novel tripodal ligands, N,N′,N′′-tri-(3′-phenylpropionic acid-2′-yl-)-1,3,5-triaminomethylbenzene (Ll), N,N′,N′′-tri-(4′-methylvaleric acid-2′-y1-)-1,3,5-triaminomethylbenzene (L2) and N,N′,N′′-tri-(3′methylvaleric acid-2′-yl-)-1,3,5-triaminomethylbenzene (L3), have been synthesized and fully characterized. The
stabilizing ability of complexes of the three ligands with transition metal ions Cu(II), Ni(II), Zn(II) and Co(II) and rare
earth metal ions La(III), Nd(III), Sm(III), Eu(III) and Gd(III) has been investigated by the pontentiometric method in water
and in aqueous KNO3 (0.1 mol dm−3) at 25.0±0.1 °C, respectively. The results show that there is a great deal of difference between two series of complexes’
stabilities. An explanation of the difference has been given. 相似文献
8.
Two multidentate ligands: N,N′-di-(propionic acid-2′-yl-)-2,9-di-aminomethylphenanthroline (L1) and N,N′-di-(3′-methylbutyric acid-2′-yl-)-2,9-di-amino-methylphenanthroline (L2) were synthesized and fully characterized by 1H NMR and elemental analysis. The binding ability of L1 and L2 to metal ions such as M(II) (M = Cu, Zn, Co and Ni) and Ln(III) (Ln = La, Nd, Sm, Eu, and Gd) has been investigated by potentiometric
titration in aqueous solution and 0.1 mol dm−3KNO3 at 25.0 ± °C. In view of the structure of L1 and L2, mononuclear metal complexes can be formed in solution. The stability constants of binary complexes of ligands L1 and L2
with metal ions M(II) and Ln(III) have been determined respectively and further discussed. 相似文献
9.
The isotopomers of L-tryptophan (L-Trp) labeled with hydrogen isotopes in the indole ring were obtained by isotope exchange
method. Heavy and tritiated water were used as the sources of stable and radioactive label. Three isotopomers, i.e., [4′-2H]-L-Trp, [4′-3H]-L-Trp, and doubly labeled [4′-2H/3H]-L-Trp were synthesized by isotope exchange enhanced by irradiation with a mercury discharge lamp. The indole whole ring
labeled isotopomers, i.e., [2′,4′,5′,6′,7′-2H5]-L-, [2′,4′,5′,6′,7′-3H5]-L-, and doubly labeled [2′,4′,5′,6′,7′-2H/3H]-L-Trp were synthesized by isotope exchange between L-Trp and D2O or DTO in the presence of deuteriated trifluoroacetic acid. 相似文献
10.
Summary. The inorganic-organic coordination polymer infin;
2[Cu2I2(μ-4-4′-bipyridine)] was prepared by the reaction of Cu(I)I and 4,4′-bipyridine in acetonitrile. Its structure consists of staircase-like CuX double chains which are connected to sheets by the 4,4′-bipyridine ligands. The thermal decomposition of the corresponding 1:1 copper(I) halide-4,4′-bipyridine compounds infin;
2[CuX(μ-4-4′-bipyridine)] (X = Cl, Br, I) was investigated using simultaneous difference thermal analysis and thermogravimetry (DTA-TG), thermomicroscopy,
and temperature resolved X-ray powder diffraction in air or argon. Upon heating infin;
2[CuX(μ-4-4′-bipyridine)], several changes in sample mass are observed which correspond to a stepwise loss of the organic ligands.
Temperature-resolved X-ray powder diffraction proves that infin;
2[CuX(μ-4-4′-bipyridine)] transforms to infin;
2[Cu2
X
2(μ-4-4′-bipyridine)] during the decomposition; the latter looses the remaining ligands when heated further, forming the corresponding
copper(I)halides. When the experiments were performed under an argon atmosphere, the 2:1 coordination polymers were obtained
as phase-pure compounds.
Received March 1, 2001. Accepted April 11, 2001 相似文献
11.
The inorganic-organic coordination polymer infin; 2[Cu2I2(μ-4-4′-bipyridine)] was prepared by the reaction of Cu(I)I and 4,4′-bipyridine in acetonitrile. Its structure consists of staircase-like CuX double chains which are connected to sheets by the 4,4′-bipyridine ligands. The thermal decomposition of the corresponding 1:1 copper(I) halide-4,4′-bipyridine compounds infin; 2[CuX(μ-4-4′-bipyridine)] (X = Cl, Br, I) was investigated using simultaneous difference thermal analysis and thermogravimetry (DTA-TG), thermomicroscopy, and temperature resolved X-ray powder diffraction in air or argon. Upon heating infin; 2[CuX(μ-4-4′-bipyridine)], several changes in sample mass are observed which correspond to a stepwise loss of the organic ligands. Temperature-resolved X-ray powder diffraction proves that infin; 2[CuX(μ-4-4′-bipyridine)] transforms to infin; 2[Cu2 X 2(μ-4-4′-bipyridine)] during the decomposition; the latter looses the remaining ligands when heated further, forming the corresponding copper(I)halides. When the experiments were performed under an argon atmosphere, the 2:1 coordination polymers were obtained as phase-pure compounds. 相似文献
12.
The basicities of several 2′-, 3′-, and 4′-substituted 4-acetylbiphenyls and biphenyl-4-carboxylic acids have been determined
spectrophotometrically in sulphuric acid media at 30°C. The pKBH
+ of 3′- and 4′-substituted compounds are correlated by the Hammett equation. The 4′-methoxy group deviates considerably in
the Hammett plot. This is attributed to its conjugative interaction with the carbonyl or carboxyl group aided by protonation.
Good correlation exists between pKBH
+ and σ+. The basicities of 2′-substituted 4-acetylbiphenyls and biphenyl-4-carboxylic acids reaffirm the existence of π-electron
steric effect of 2′substituents. 相似文献
13.
Meryem Çamur 《Journal of organometallic chemistry》2010,695(1):45-227
The phthalonitrile derivative chosen for the synthesis of substituted phthalocyanines [M: 2H, Zn(II), Co(II)] with four chloro and four phenyloxyacetic acid substituents on the periphery is 4-chloro-5-(4-phenyloxyacetic acid)phthalonitrile. The sodium salt of carboxyl substituted zinc phthalocyanine is good soluble in water. Further reactions of zinc and cobalt phthalocyanines bearing phenyloxyacetic acid with thionylchloride gave the corresponding acylchlorides. This functional group reacted with hydroxymethylferrocene in dry DMF to obtain ferrocenyl substituted phthalocyanines. Also chloro substituent in new phthalonitrile was substituted with hexylsulfanyl substituent and its cyclotetramerization in the presence of Zn(AcO)2·2H2O and 2-(dimethylamino)ethanol resulted with zinc phthalocyanine. The compounds have been characterized by elemental analysis, MALDI-TOF mass, FT-IR, 1H NMR, UV-Vis and fluorescence data. Aggregations properties of phthalocyanines were investigated at different concentrations in tetrahydrofuran, dimethylformamide, dimethylsulfoxide, water, and water/ethanol mixture. Also fluorescence spectral properties are reported. 相似文献
14.
Two long-chain multidentate ligands: 2,9-di-(n-2′,5′,8′-triazanonyl)-1,10-phenanthroline (L1) and 2,9-di-(n-4′,7′,10′-triazaundecyl)-1,10-phenanthroline (L2) were synthesized. The hydrolytic kinetics of p-nitrophenyl phosphate (NPP) catalyzed by complexes of L1 and L2 with La(III) and Gd(III) have been studied in aqueous solution at 298 K, I = 0.10 mol · dm−3 KNO3 at pH 7.5–9.1, respectively. The study shows that the catalytic effect of GdL1 was the best in the four complexes for hydrolysis
of NPP. Its kLnLH−1, k
LnL and pK
a are 0.0127 mol−1 dm3 s−1, 0.000022 mol−1 dm3 s−1 and 8.90, respectively. This paper expounds the result from the structure of the ligands and the properties of the metal
ions, and deduces the catalysis mechanism. 相似文献
15.
Desigan Reddy Kate J. Akerman Matthew P. Akerman Deogratius Jaganyi 《Transition Metal Chemistry》2011,36(6):593-602
The substitution kinetics of the complexes [Pt(terpy)Cl]Cl·2H2O (PtL1), [Pt(tBu3terpy)Cl]ClO4 (PtL2), [Pt{4′-(2′′′-CH3-Ph)terpy}Cl]BF4 (PtL3), [Pt{4′-(2′′′-CF3-Ph)terpy}Cl]CF3SO3 (PtL4), [Pt{4′-(2′′′-CF3-Ph)-6-Ph-bipy}Cl] (PtL5) and [Pt{4′-(2′′′-CH3-Ph)-6-2′′-pyrazinyl-2,2′-bipy}Cl]CF3SO3 (PtL6) with the nucleophiles imidazole (Im), 1-methylimidazole (MIm), 1,2-dimethylimidazole (DIm), pyrazole (Pyz) and 1,2,4-triazole
(Trz) were investigated in a methanolic solution of constant ionic strength. Substitution of the chloride ligand from the metal
complexes by the nucleophiles was investigated as a function of nucleophile concentration and temperature under pseudo first-order conditions using UV/Visible and stopped-flow spectrophotometric techniques. The reactions follow the rate law
k\textobs = k2 [ \textNu ] + k - 2 k_{\text{obs}} = k_{2} \left[ {\text{Nu}} \right] + k_{ - 2} . The results indicate that changing the nature or distance of influence of the substituents on the terpy moiety affects the
π-back-donation ability of the chelate. This in turn controls the electrophilicity of the metal centre and hence its reactivity.
Electron-donating groups decrease the reactivity of the metal centre, while electron-withdrawing groups increase the reactivity.
Placing a strong σ-donor cis to the leaving group greatly decreases the reactivity of the complex, while the addition of a good π-acceptor group significantly
enhances the reactivity. The results indicate that the metal is activated differently by changing the surrounding atoms even
though they are part of a conjugated system. It is also evident that substituents in the cis position activate the metal centre differently to those in the trans position. The kinetic results are supported by DFT calculations, which show that the metal centre is less electrophilic when
a strong σ-donor is cis to the leaving group and more electrophilic when a good π-acceptor group is part of the ring moiety. The temperature dependence
studies support an associative mode of activation. An X-ray crystal structure of Pyz bound to PtL3 was obtained and confirmed
the results of the DFT calculations as to the preferred N-atom as a binding site. 相似文献
16.
N. M. Logacheva V. E. Baulin E. N. Pyatova I. S. Ivanova A. Yu. Tsivadze 《Russian Journal of Coordination Chemistry》2009,35(9):648-656
Complexes of Co(II), Ni(II), Zn(II), and Cu(II) perchlorates and hexafluorophosphates with 4′-(4″-benzo-15-crown-5)oxy-2,2′:6′,2″-terpyridine
(L) [M(L)2](ClO4)2 · 3H2O and [M(L)2](PF6)2 · 2H2O were synthesized. The spectral criteria of ligand coordination through the terpyridine nitrogen atoms were established.
An assumption concerning the benzo-15-crown-5 conformation in the ligand molecule in the synthesized complexes was made. The
extraction and ion-selective properties of L were studied. 相似文献
17.
Abstract Two new Keggin-polyoxometalate hybrids, {[Cu2(4,4′-bpy)2][PW10VIW2VO40]}[Cu2(obpy)2]4 · 2 H2O (1) and {[Cu4(2,2′-bpy)4(4,4′-bpy)3][SiW12O40]} · 2H2O (2) (4,4′-/2,2′-bpy = 4,4′-/2,2′-bipyridyl, Hobpy = 6-hydroxy-2,2′-bipyridyl), were hydrothermally synthesized and structurally
characterized. Gillard type hydration of 2,2′-bipy is observed during the synthesis of 1, resulting in a new obpy ligand in situ. X-ray structural analyses show that 1 consists of 1D hybrid chain {[Cu2(4,4′-bpy)2][PW10VIW2VO40]}∞ and [Cu2(obpy)2] dimer, whereas 2 possesses 1D hybrid structure based on Keggin-type [SiW12O40]4− anions and tetra-nuclear copper complexes [Cu4(2,2′-bpy)4(4,4′-bpy)3]4+. Both compounds present interesting supramolecular architectures based on π–π stacking and hydrogen bonds.
Graphical Abstract Compounds {[Cu2(4,4′-bpy)2][PW12O40]}[Cu2(obpy)2]4 · 2H2O (1) and [Cu4(2,2′-bpy)4(4,4′-bpy)3][SiW12O40] · 2H2O (2) were hydrothermally synthesized. 1 features that the [Cu2(obpy)2] dimers based on in situ generated obpy ligands are stumped between the layers where 1D hybrid chain {[Cu2(4,4′-bpy)2][PW12O40]}∞ locates, while 2 exhibits 1D chain-like structure based on anions [SiW12O40]4− and tetra-copper complexes [Cu4(2,2′-bpy)4(4,4′-bpy)3]4+.
相似文献
18.
The new metallophthalocyanine (Zn, Cu, Ni, Co) polymers containing 4,6,10,12,16,18,22,24-octakis(2-hydroxyethoxy)-2,8,14,20-tetramethylresorcinarene are described. Firstly, 4,6,10,12,16,18,22,24-octakis(2-hydroxyethoxy)-2,8,14,20-tetramethylresorcinarene compound (1) was synthesized by treating resorcinarene with 2-chloroethanol under microwave irradiation. Then, tetrakis(4,5-bis(2-hydroxyethoxy))phthalonitrile substituted resorcinarene compound (2) and octakis(4-(2-hydroxyethoxy))phthalonitrile substituted resorcinarene compound (3) were synthesized by treating compound (1) with 4,5-dichloro-1,2-dicyanobenzene and 4-nitro-1,2-dicyanobenzene, respectively, under microwave irradiation. The chlorides Cu (II), Ni (II), Co (II), were employed in order to synthesize the corresponding metallophthalocyanine polymers (2b–d and 3b–d) and Zn(CH3COO)2 was used for the preparation of zinc phthalocyanine polymers (2a and 3a). All products were synthesized by microwave-assisted synthesis method. The structures were characterized by elemental analyses, 1H NMR, 13C NMR, UV–Vis and FTIR spectroscopy. 相似文献
19.
A new chromone-substituted dihydrotriflavonol, (2S,3S)[6-{(3S) 3″,5″-dihydroxy-6″-methoxydihydrochromone}5,3′,4′,5′-tetrahydroxy-7-methoxy-3-O-8-dihydroflavone]2 3-O-8[6-{(3S) 3″,5″-dihydroxy-6″methoxydihydrochromone}3,5,3′,4′,5′-pentahydroxy-7-methoxydihydroflavonol] was isolated from the leaves
of Anogeissus pendula. The structure was determined by UV, 1H NMR, 13C NMR, HMBC, and CD data. 相似文献
20.