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1.
Homobinuclear complex (HCuL)2 (1) (H3L: N-3-carboxylsalicylidene-N'-salicylaldehyde-1,2-diaminoethane) was obtained from self-organization of the reported complex HCuL, and its crystal structure was determined through X-ray diffraction at room temperature. The crystal of complex 1 belongs to monolinic system, the space group Cc, a=2.5326(5) nm, b=0.88861(18) nm, c=1.3738(3) nm, β=96.95(3)°, Z=4, R1=0.0520, wR2=0.1185. (HCuL)2 is a dimeric molecule and has extended phenolic oxygen-bridged structure. In addition, using mononuclear complex HCuL as building blocks, Cu(Ⅱ)-Mg(Ⅱ)-Cu(Ⅱ) heterotrinuclear complex 2 was synthesized, and its crystal structure also has been determined by X-ray analysis. The crystal of complex 2 is of monoclinic system, space group Pc, a=1.1816(2) nm, b=1.5599(3) nm, c=1.9642 (4) nm, β=98.22°, Z=2, R1=0.0701, wR2=0.1498. Each dissymmetricai cell unit of complex 2 contains two heterotrinucler neutral molecules: {[CuL(H2O)]Mg[CuL(CH3OH)]} and {[CuL]Mg[CuL(H2O)]}. 相似文献
2.
Synthesis, Characterization and Properties of Tri-substitute Potassium Salt of Trinitrophloroglucinol 总被引:1,自引:0,他引:1
The title complex [K3(TNPG)·(H2O)2]n was synthesized by the reaction of the aqueous solutions of trinitrophlomglucinol (TNPG) with KHCO3. The complex was characterized by elemental analysis and FTIR spectroscopy, and its single crystal structure was determined by X-ray diffraction analysis. The structural analysis demonstrates that two different coordination modes of K cations [K(1) and K(2)] are around TNPG^3- anions in complex [Ka(TNPG)·(H2O)2]n, where the coordination numbers are eight. All K atoms coordinate with O atoms of phenolic hydroxyl group and nitro-group simultaneously. The thermolysis of the [Ka(TNPG) · (H2O)2]n has been investigated by using differential scanning calorimetry (DSC) and thermogravimetry-derivative thermogravimetry (TG-DTG) at a heating rate of 10 ℃/min. The thermal decomposition processes of the title complex were comprised of one endothermic dehydration stage and one exothermic decomposition stage in 270-320℃, and the final decomposition residue contained KNC. Impact and friction sensitivity results of the complex revealed its sensitive nature towards mechanical stimuli. The experiments verified that the complex has some characteristics of explosive. 相似文献
3.
A new dinuclear complex, [Ag(L)(CH3CN)]2(ClO4)2·2H2O(L=2,3-di-2-pyridylquinoxaline), was prepared and characterized by elemental analyses, IR spectroscopy, and single-crystal X-ray diffraction analyses. The interaction of the complex with calf thymus DNA(CT-DNA) was investigated by absorption, fluorescence spectroscopies, and viscosity measurement. The results suggested that the complex was bound to DNA via an intercalative mode. The intrinsic binding constant value Kb was found to be approximately 1.48×10^3 L·mol^-1. Moreover, the Ag(I) complex could cleave the plasmid pUC19 DNA from the supercoiled Form Ⅰto the nicked FormⅡ under irradiation at 365 nm. 相似文献
4.
A new nickel(II) complex [NiL2](DMF)4 (HL = 2'-[4-N,N'-(dimethylamino- benzylidene)]-3,5-dihydroxybenzoylhydrazide) has been synthesized and its structure was characterized by IR,UV-Vis,1H NMR and elemental analysis. The fluorescence emission mechanism of the complex was discussed by fluorimetric spectra. The single-crystal structure was determined by X-ray diffraction analysis. The crystal belongs to the triclinic system,space group P1 with a = 0.9918(4),b = 1.1297(4),c = 1.1331(4) nm,α = 76.860(7),β = 75.105(6),γ = 89.022(7)°,V = 1.1936(8) nm^3,Z = 1,μ = 0.472 mm^-1,Dc = 1.319 g/cm^3,F(000) = 502 and Rint = 0.0913. In the title compound,the nickel(II) atom is four-coordinated with two nitrogen atoms from amide and two oxygen atoms from keto group. The complex is centrosymmetric with nickel located at the center. 相似文献
5.
HAN Qiu-xia ;WANG Chun-zhang ;Institute of Molecular Crystal Engineering School of Chemistry Chemical Engineering Henan University Kaifeng P R. China ;NIU Jing-yang ;WANG Jing-ping 《高等学校化学研究》2008,24(3):255-259
The reaction of α-H3[PW12O40] with Y(NO3)3 in the presence of DMF or DMSO leads to two complexes with the formulae {Y(DMSO)7}·PW12O40(1) and {[Y(DMF)7]2PW12O40}·PW12O40(2). The crystal structures indicate that complex 1 consists of discrete [YLn]3+ cations and α-Keggin heteropolyanions [PW12O40]3-, whereas, in complex 2, donor-acceptor interaction results in a cation-anion-cation triplet. In addition, the electrochemical behavior of the two complexes indicates the usual successive reduction processes of the W atoms in the anions. 相似文献
6.
A newly synthesized aromatic sulfonate compound,complex 2 with formula of K2[H3COOC-C6H3(SO3)2]·2H2O(methyl 3,5-disulfo-benzoate dipotassium dihydrate) was synthesized and characterized by elemental analysis,infrared(IR) spectrometry,nuclear magnetic resonance(NMR) and crystal structure measurement.Single-crystal X-ray diffraction(XRD) revealed that complex 2 crystallized in the triclinic system with space group P(i).Complex 2 was used as nucleating agent for poly(L-lactide)(PLLA).The crystallization of PLLA with powder of complex 2 was investigated by means of differential scanning calorimetry(DSC) and polarized optical microscopy (POM).The results prove that complex 2 was effective as nucleating agent for PLLA.It could accelerate crystallization by reducing the induction time and increasing the density of nuclei in the crystallization process.The half-time of crystallization(t0.5) for pure PLLA was about 8 times longer than that of PLLA sample with 1.0%(mass fraction) of complex 2. 相似文献
7.
The unsymmetric precursor ethyl 6-acetylpyridine-2-carboxylate (4) was synthesized from 2,6-dimethylpyridine (1). On the basis of this precursor, a new mono(imino)pyridine ligand (5) and the corresponding Co(Ⅱ) complex {2-carbethoxy-6-[1-[(2,6-diethylphenyl)imino]ethyl]pyridine}CoCl2 (6) were prepared. The crystal structure of complex indicates that the 2-carbethoxy-6-iminopyridine is coordinated to the cobalt as a tridentate ligand using [N, N, O] atoms, and the coordination geometry of the central cobalt is a distorted trigonal bipyramid, with the pyridyl nitrogen atom and the two chlorine atoms forming the equatorial plane. Being applied to the ethylene oligomedzation, this cobalt complex shows catalytic activity of 1.820× 10^4 g/mol-Cooh at 101325 Pa of ethylene at 15.5℃ for 1 h, when 1000 equiv, of methylaluminoxane (MAO) is employed as the cocatalyst. 相似文献
8.
A homodinuclear complex (NH3CH2CH2CH2NH3)2 {Na2[(C6H4O2)2] (C6H4O2H)2} (1) has been synthesized by a solution-based self-assembly route. It crystallized in monoclinic system with space group P21/c. Every sodium ion coordinates in a tetragonal prism fashion with two O atoms of a terminal chelating catecholate ligand and three O atoms from two bridging catecholate ligands. Two neighboring NaO5 tetragonal prisms are edge-shared and centrosymmetric with regard to the inversion center to form a binuclear cluster {Na2[(C6H4O2)2](C6H4OOH)2}^4- anion. The complex anions were aligned parallelly by n-n interaction and linked with the protonated 1,3-propylenediamine through hydrogen bonds which were assembled into a multi-lamellar structure with channels. The crystal exhibits rectangular geometry with an interior triangle hollow structure under optical microscopy. And the scanning electron microscopy (SEM) indicates that the wall of the tubes shows multi-lamella morphologies. Further, the transmission electron microscopy (TEM) reveals that the crystal is composed of multi-lamellar nano-tubes with diameters less than 100 nm. The molecular structure of the complex was compared with that of its isomer complex 2. 相似文献
9.
CHEN Jun XU Xing-You GAO Jian LI Yan-Hui XU Guo-Xiang 《结构化学》2007,26(6):632-636
A new mononuclear [Zn(H-1L)2] (L = 1H-indole-3-ethylene-salicylaldimine) was synthesized through the reaction of Zn(Ac)2, salicylaldehyde and tryptamine in hot ethanol solution and characterized by X-ray crystal structure analysis. The crystal belongs to monoclinic, space group P21/n with a = 15.014(2), b = 10.857(1), c = 17.489(1)A,β = 95.49(1)°, V = 2837.8(5) A^3, Z = 4, Dc = 1.386 g/cm^3, μ = 0.904 mm-1, F(000) = 1232, the final R = 0.0463 and wR = 0.0890 for 4990 independent reflections. In the complex, the Zn2+ ion presents a distorted N2O2 tetrahedral coordination involving two H-1L ligands. 相似文献
10.
A manganese(Ⅱ) complex (tataH)2[Mn(pydc)2]·4H2O (C20H28MBN14O12, Mr = 711.50, tata = 2,4,6-triamino-1,3,5-triazine, pydcH2 = pyridine-2,6-dicarboxylic acid) has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group P1^-, with a = 9.9847(3), b = 10.9813(3), c = 15.2616(5)A, a = 101.5310(10), β = 90.2610(10), γ = 116.4600( 10)% V = 1459.44(8)A^3, Z = 2, Dc = 1.619 g/cm^3,μ = 0.539 mm^-1, F(000) = 734, the final R = 0.0292 and wR = 0.0745. In the crystal the Mnn atom is six-coordinated by four carbonyl oxygen atoms and two pyridine nitrogen atoms from two tridentate pydc ligands to furnish a distorted octahedral geometry. The complex shows the A…D…D'…A' H-bonded tetramer. The molecules are packed in a three-dimensional framework structure by the combination of O-H…O, N-H…O and N-H…N hydrogen bonds between (tataH)^+, [Mn(pydc)2]^2- and crystal water. 相似文献
11.
Eric W. Ainscough Andrew M. Brodie Andreas Derwahl Graham H. Freeman Carl A. Otter 《Polyhedron》2007,26(18):5398-5405
The reaction of 1,2-bis(diphenylthioylphosphino)hydrazine (L) with copper(I) and mercury(II) halides affords the complexes, [{CuLX}2] (X = I, Br or Cl), [HgLX2] (X = Cl or Br) and the tetrametallic complex, [{L(HgI2)2}2]. Single crystal X-ray structures have been performed on the uncoordinated ligand, L, as well as the complexes [{CuLX}2] (X = I, Br and Cl), [HgLBr2] and [{L(HgI2)2}2. The molecules of L exist as dimers as a result of pairs of N–HS hydrogen bonds. The copper(I) complexes are centrosymmetric dimetallic species, the two copper atoms being bridged by L and the X atoms. In all cases the coordination sphere around the Cu atoms is approximately trigonal pyramidal with an ‘S2X2’ donor set. The complex, [HgLBr2], is a distorted tetrahedral monomer with an ‘S2Br2’ donor set and L acting as a bidentate thus forming a seven-membered chelate ring. The tetramercury iodo complex, [{L(HgI2)2}2], contains two ‘L(HgI2)2’ units linked centrosymmetrically via an I atom from each moiety. The geometry around the Hg atoms is distorted tetrahedral. The influence of hydrogen bonding between the hydrazine backbone hydrogens of L and the coordinated halide ions in for the structures of the metal complexes is discussed. 相似文献
12.
Jose Vicente Maria-Teresa Chicote Maria D. Bermudez M. J. Sanchez-Santano 《Journal of organometallic chemistry》1986,310(3):401-409
The reaction (1 : 1) between [A
Me2)Cl2] and [Hg(2-C6H4-N=NPh)2] gives the complex [(2-PhN=NC6H4)A
MeC2)Cl], which on treatment with AgClO4 gives [(2-Ph
Me2)]ClO4. From this complex, the species [(2-PhN=NC6H4)A
Me2)X] (X = CH3COO, CN), or [(2-PhN=NC6H4)A
Me2)L] (L = PPh3, py) are obtained by reaction with the corresponding KX salts or neutral ligands.
The crystal structure of [(2-Ph Me2)][AuCl4] (obtained by metathesis between the corresponding perchlorate and tetramethylammonium salts) has been determined; the cation displays square-planar coordination with two cis-nitrogen (Au---N: 2.166(15), 2.140(14) Å) and two cis-carbon (Au---C: 2.021(16), 2.033(17) Å) atoms bonded to the gold atom. 相似文献
13.
A novel Pt(Ⅱ)-based metallointercalator terpyridine complex linked with a 2, 2, 6, 6-tetramethyl-1-piperidinyl N-oxide (TEMPO) derivative was prepared by a reaction between 4'-TEMPO-terpyridine (L) and a Pt(Ⅱ) salt. This complex presented unusual luminescence quenching owing to the effect of the stable nitroxide radical. The crystal structure of[Pt(terpy-TEMPO)Cl]Cl·H2O·CH3OH (terpy=2, 2':6', 2"-terpyridine) was elucidated by X-ray crystallography. Additionally, the effect of TEMPO on the photophysical properties of[Pt(terpy-TEMPO)Cl] Cl·H2O·CH3OH was investigated by UV-Vis, fluorescence emission, and electron paramagnetic resonance (EPR) spectroscopy. Data from the absorption and luminescence properties (298 K) of the[Pt(terpy-TEMPO)Cl]+ complex indicated the presence of two groups of typical bands:an intense band B with distinct vibronic structures (270-350 nm, ε>104 dm3·mol-1·cm-1) and a less intense band A (370-450 nm, ε~103 dm3·mol-1·cm-1). These two bands are generally assigned to ligand-to-ligand charge transfer (LLCT) and metal-to-ligand charge transfer (MLCT) excited states, respectively. Furthermore, efficient photoluminescent quenching behavior was observed in the emission spectra of this complex system. Quantum calculations of the molecular energy gaps and bands were performed by Gaussian 09 software. The calculated results verified that TEMPO greatly affects the energy gaps between the highest occupied molecular orbital and the lowest unoccupied molecular orbital. Thus, the relationship between efficient photoquenching and molecular structure was theoretically interpreted. EPR results indicated that when TEMPO is attached to a macrocyclic terpyridine platinum complex, e.g., [Pt(terpy)Cl]+, the terpyridine platinum complex does not affect the hyperfine coupling constant (A value) and g factor (g values) but the rotation and relaxation times of the TEMPO radical. 相似文献
14.
The reduction of colourless [LReVIIO3]Br in an acetone-water mixture (6: 1) with zinc amalgam affords green, air-sensitive [LReVO2Br] which forms a violet complex [LReO(μ-O)2ReOBr2]in aqueous solution (L = 1,4,7-triazacyclononane; C6H15N3). From a similar reduction of [LReO3]ReO4 the violet neutral complex [LReO(μ-O)2ReO(ReO4)2] was obtained. [LReO3]+ is deprotonated in alkaline solution (pKa = 10.3 + 0.2, 25°C) and [(C6H14N3)ReO3] was isolated as a yellow solid. The latter amido rhenium(VII) compound reacted in dimethylformamide with R---X (R = CH3, benzyl; X = Cl), affording at the cyclic amine, N,N′,N″-trisalkylated complexes of the type [L′ReO3]X. The monomeric rhenium(V) complexes [LReOX2]X (X = Cl, Br, I) were obtained from the reaction of [n-Butyl4N]ReOX4 and L in acetonitrile. IR, UV-vis, 17O NMR spectra of these compounds are reported. 相似文献
15.
The dinuclear μ-oxomolybdenum(V) complexes [Mo2O3(PyS)4] (1), [Mo2O3(PySe)4] (2) and [Mo2O3(4-CF3-PymS)4] (3) were obtained by similar reactions of the [MoO2Cl2(DME)] precursor with the corresponding heterocyclic bidentate (N,X) ligands, X = S, Se, where PyS, PySe and 4-CF3-PymS are the anions of pyridine-2-thione, pyridine-2-selenolato and 4-trifluoromethyl-2-pyrimidinthiol, respectively. All compounds were characterized by elemental analysis, IR, NMR, EI-MS spectroscopy and X-ray diffraction. The crystal structures of 1–3 all include the common [Mo2O3]4+ core. Compounds 1 and 2 are isostructural. The catalytic oxo-transfer properties of the molybdenum(V) compounds 1 and 2 were studied by the use of PPh3 in DMSO with a considerably higher catalytic activity for the thionato containing complex 1 than for its selenolato containing analogue 2. 相似文献
16.
Ritu Bala Raj Pal Sharma Paloth Venugopalan William T.A. Harrison 《Journal of Molecular Structure》2007,830(1-3):8-13
In an effort to utilize the [Co(NH3)6]3+ cation as a new anion receptor (binding agent) for dihydroxy dicarboxylate anion i.e., tartrate, orange single crystals of hexaamminecobalt(III) chloride (R,R)-tartrate monohydrate, [Co(NH3)6]Cl(C4H4O6)·H2O, were obtained by reacting hexaamminecobalt(III) chloride with potassium–sodium tartrate tetrahydrate in a 1:1 molar ratio in hot water. The single crystal X-ray structure determination of [Co(NH3)6]Cl(C4H4O6)·H2O revealed that a distinctive network of hydrogen bonding interactions (N–HO, N–HCl−, O–HO) stabilize the crystal lattice. This is the first complex salt of hexaamminecobalt(III) with dihydroxy dicarboxylate anion i.e., tartrate. 相似文献
17.
Bis(5-methyl-2-(2,3-diaza-4-(5-methyl-2-thienyl)buta-1,3-dienyl)thiophene) silver(I) complex was synthesized in high yield by refluxing 5-methyl-2-(2,3-diaza-4-(5-methyl-2-thienyl)buta-1,3-dienyl)thiophene (L) with silver nitrate or silver perchlorate in anhydrous acetonitrile. The product thus formed was well characterized by NMR, IR, UV–Vis and mass spectroscopies as well as elemental analysis and electrochemical analysis. Molecular structures of compounds L, [L2Ag]NO3 and [L2Ag]ClO4 were determined by single crystal X-ray diffraction analysis. It was found that the C=N double bond of the ligand rotated during the course of ligand coordination in the case of the perchlorate salt but not in the case of the nitrate salt. 相似文献
18.
Milan Maji Mossaraf Hossain Madhumita Chatterjee Shyamal Kumar Chattopadhyay Vedavati G. Puranik Pinak Chakrabarti Saktiprosad Ghosh 《Polyhedron》1999,18(27):1436-3739
Reaction of Ru(PPh3)2Br2 with the NNS chelating tridentate ligand 2-pyridyl-N-(2′-methylthiophenyl)methyleneimine (L) led to the isolation of the ruthenium(II) complex [Ru(L)(PPh3)Br2]. Reactivity of this complex with different bidentate chelating ligands revealed that the products are quite different from those obtained by reacting Ru(L)(PPh3)Cl2 (the corresponding cis dichloro complex) with the same ligands under comparable conditions. The mixed chelates were isolated and characterised by elemental analysis, magnetic moment measurement and by different spectroscopic methods along with their precursor. Electrochemistry of the complexes was examined by cyclic voltammetry using a platinum working electrode and a Ag/AgCl electrode as reference. The crystal structure of [Ru(L)(PPh3)Br2] disclosed that, unlike Ru(L)(PPh3)Cl2, the two bromo ligands are in trans position and this explained the difference in its reactivity pattern from the corresponding chloro complex. 相似文献
19.
Alexander J. Blake Robert O. Gould Alan J. Holder Aidan J. Lavery Martin Schr der 《Polyhedron》1990,9(24):2919-2924
Reaction of [18]aneS6 with two molar equivalents of [Cu(NCMe)4](ClO4) in CH2Cl2-MeCN affords the binuclear copper(I) complex [Cu2([18]aneS6)(NCMe)2](ClO4)2. The single crystal X-ray structure of the complex shows a centrosymmetric cation with two tetrahedral copper(I) centres each coordinated to three thioether S-donors of [18]aneS6,Cu---S(1) = 2.3200(15), Cu---S(4) = 2.3415(16), Cu---S(7) = 2.3250(15) Å, and to one MeCN molecule, Cu---N(1) = 1.939(5) Å, to give an overall NS3-donation at the metal centres. Additionally, S(7′) shows a long-range interaction, Cu …S(7′) = 3.318(2) Å thus distorting the coordination geometry of the metal ion towards trigonal bipyramidal. The metal-metal separation of 4.428(2) Å suggests that there is no significant interaction between the copper centres of the dimer. Reaction of [9]aneS3 with one molar equivalent of [Cu(NCMe)4](ClO4) in refluxing MeCN in the presence of ligands, L, affords the adducts [Cu([9]aneS3)L]+ (L = PPh3, AsPh3). The single crystal X-ray structure of the complex [Cu([9]aneS3)(AsPh3)](ClO4) shows tetrahedral AsS3 coordination at copper(I) with [9]aneS3 bound facially to the metal centre, Cu---S = 2.303(6), Cu---As = 2.322(4) Å. 相似文献
20.
The synthesis and crystal structures of three ytterbium(III) complexes of homoazacalixarenes are reported. In all cases, the complexes are obtained without addition of a base, the protons of the complexing phenolic moieties being transferred to the amine groups upon complexation. The 1:1 complex between p-chloro-N-benzylhexahomotriazacalix[3]arene (1) and Yb(NO3)3 is analogous to the neodymium(III) complex reported previously, with the metal ion bound to three phenoxide groups and three nitrate ions. A second 1:1 complex is obtained with Yb(NO3)3 and p-methyl-N-benzyltetrahomodiazacalix[4]arene (2), in which the metal ion is bound to two phenoxide groups only. The replacement of nitrate by triflate counter-ions results in the formation of a 1:2 ‘sandwich’ complex with 1, in which two divergent calixarene molecules are bridged by the metal ion, the counter-ions being non-bonding. 相似文献