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1.
Montserrat Lpez‐Deber Rufina Bastida Maria del Carmen Fernndez‐Fernndez Alejandro Macías Adolfo Rodríguez Laura Valencia 《无机化学与普通化学杂志》2005,631(11):2033-2040
A new mixed oxaaza‐macrocyclic ligand, L1, has been obtained by direct synthesis between 1,4‐bis‐(2′‐formylphenyl)‐1,4‐dioxabutane and the diamine 2,2′‐ethylenedioxydiethylamine. The dialkylated ligand L2, bearing two nitrobenzyl pendant groups, has been prepared and transitional, post‐transitional and Ca2+, Sr2+, and Ba2+ metal complexes have been synthesized in order to elucidate the coordination preferences. The crystal structures of the ligands L1 and L2 and the complexes [SrL2(H2O)2](ClO4)2 and [BaL2(NCS)2(CH3CN)]·CH3CN have been determined by single crystal X‐ray diffraction. The structures reveal the presence of mononuclear endomacrocyclic complexes where the pendant arms radiate away from the ligand. 相似文献
2.
Jesús Martínez Rufina Bastida Alejandro Macías Laura Valencia Manuel Vicente 《无机化学与普通化学杂志》2005,631(11):2046-2053
The pendant‐armed ligands L1 and L2 were synthesized by N‐alkylation of the four secondary amine groups of the macrocyclic precursor L using o‐nitrobenzylbromide (L1) and p‐nitrobenzylbromide (L2). Nitrates and perchlorates of CuII, NiII and CoII were used to synthesize the metal complexes of both ligands and the complexes were characterized by microanalysis, MS‐FAB, conductivity measurements, IR and UV‐Vis spectroscopy and magnetic studies. The crystal structures of L1, [CuL1](ClO4)2·CH3CN·H2O, [CuL2](ClO4)2·6CH3CN, [CuL2][Cu(NO3)4]·5CH3CN·0.5CH3OH and [NiL2](ClO4)2·3CH3CN·H2O were determined by single crystal X‐ray crystallography. These structural analysis reveal the free ligand L1, three mononuclear endomacrocyclic complexes {[CuL1](ClO4)2·CH3CN·H2O, [CuL2](ClO4)2·6CH3CN and [NiL2](ClO4)2·3CH3CN·H2O} and one binuclear complex {[CuL2][Cu(NO3)4]·5CH3CN·0.5CH3OH} in which one of the metals is in the macrocyclic framework and the other metal is outside the ligand cavity and coordinated to four nitrate ions. 相似文献
3.
Jesús Martínez Laura Valencia Rufina Bastida David E. Fenton Sharon E. Spey Alejandro Macías 《无机化学与普通化学杂志》2002,628(5):1059-1067
The pendant‐armed ligands L1 and L2 were synthesized by N‐alkylation of the two secondary aminic groups of the oxaazamacrocyclic precursor L with o‐nitrobenzylbromide (L1) or p‐nitrobenzylbromide (L2). Metal complexes of L1 and L2 have been synthesized and characterized by microanalysis, MS‐FAB, conductivity measurements, IR, UV‐Vis, 1H and 13C NMR spectroscopy and magnetic studies. Crystal structures of ligands L1 and L2, as well as complexes [CdL1(NO3)2]·2CH3CN and [Ag2Br(L2)2](ClO4)·2CH3CN have been determined by single crystal X‐ray crystallography. 相似文献
4.
Nickel(II), Cadmium(II), and Copper(II) Complexes Based on Ditopic Terpyridine Derivative Ligand: Syntheses,Crystal Structures,and Luminescent Properties
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Ai‐Jiang Zhang Chang‐Juan Chen Dong‐Yang Lou Yu‐Hang Miao Chen‐Xu Qiao Jiang‐Bo Hu 《无机化学与普通化学杂志》2016,642(14):817-822
Three complexes with the ditopic ligand 4′‐[4‐(quinolin‐8‐yloxymethyl)phenyl]‐2,2′:6′,2′′‐terpyridine (abbreviated as L ), [Ni(L)2](CH3COO)2 ( 1 ), [Cd(L)2](ClO4)2 ( 2 ), and [Cu2(L)2](ClO4)4 · 4DMF ( 3 ), were synthesized and characterized by elemental analysis, IR spectroscopy, and structurally analyzed by X‐ray single‐crystal diffraction. Interestingly, in complexes 1 and 2 , two ligands adopt a tridentate chelating pattern where the oxaquinoline group is non‐coordinated and coordinate with one MII ion (M = Ni for 1 , M = Cd for 2 ) to form a mononuclear unit. In complex 3 , two ligands bridge two CuII ions by pyridyl N atoms, ethereal O atoms, and quinolyl N atoms in a head‐to‐tail mode to generate a dinuclear [Cu2L2] unit. Moreover, extended 1D and 2D supramolecular architectures are further constructed in 1 – 3 by multiple secondary interactions such as aromatic stacking and hydrogen bonding. Notably, the structural diversity of complexes 1 – 3 can be properly assigned to the central metal ions that have distinct coordination preferences. In addition, luminescent properties of the ligand and complex 2 were also investigated. 相似文献
5.
A novel double helical dicopper(II) complex was synthesized by reaction of a polydentate ligand L = 2,2′‐bipyridyl‐6,6′‐bis(2‐acetylpyrazinohydrazone) with copper(II) perchlorate in CH3CN. The self‐assembling process was studied by UV‐Vis spectrometric titration experiments which revealed the formation of dinuclear complexes [Cu2L2](ClO4)4. The structure of dicopper double‐helicate was confirmed by X‐ray diffractometry. Each copper(II) center occupies a distorted octahedral environment. Variable‐temperature magnetic measurements reveal weak antiferromagnetic interactions between Cu(II) ion centers with J = ?0.63 cm?1. 相似文献
6.
Rainer Mattes Christoph Mühlenbrock Katharina Leeners Claudia Pyttel 《无机化学与普通化学杂志》2004,630(5):722-729
Metal Complexes with N2O2S2 Donor Set. Synthesis and Characterization of the Cobalt(II), Nickel(II), and Copper(II) Complexes of a 15‐ and a 16‐Membered Bis(2‐hydroxyethyl) Pendant Macrocyclic Ligand The macrocyclic ligands 6, 10‐bis(2‐hydroxyethyl)‐7, 8, 9, 11, 17, 18‐hexahydro‐dibenzo‐[e, n][1, 4, 8, 12]‐dithiadiaza‐cyclopentadecine ( 1 ) (L1) and 5, 13‐bis(2‐hydroxyethyl)‐7, 8, 9, 10, 16, 17, 18, 19, 20‐nonahydro‐dibenzo‐[g, o][1, 9, 5, 13]‐dithiadiaza‐cyclohexadecine (L4) have been prepared. They form the stable complexes [CoL1(‐H)CoL1](ClO4)3 ( 2 ), [NiL1](ClO4)2·MeOH ( 3 ), Λ‐[CuL1](ClO4)2·MeOH ( 4a ) and rac‐[CuL1](ClO4)2·MeOH ( 4b ), [NiL4](ClO4)2 ( 5 ), and [CuL4](ClO4)2 ( 6 ). The compounds 1 to 6 have been characterized by standard methods and single‐crystal X‐ray diffraction. In the complexes 2 to 6 the metal atoms are octahedrally coordinated by the N2O2S2 donor set of the ligands. L1 and L4 are folded herein along the N···M···S‐ and the N···M···N′‐axes, respectively. This results at the metal atom in a all‐cis‐configuration for the complexes of L1 and a trans‐N2‐cis‐O2‐cis‐S2‐configuration for the complexes of L4. The cobalt(II) complex 2 is a dimer, bridged by a rather short hydrogen bridge of 2.402(12)Å length. The copper(II) complexes of L1 and L4 differ with respect to the Jahn‐Teller‐distortion. 相似文献
7.
The syntheses of dinuclear calcium perchlorate and/or nitrate complexes by template and direct methods, employing macrocyclic ligands with 18, 20, 22, and 26 membered rings are reported. The presence of pendant arms provide with coordinative NxOy donor atoms in the smaller macrocycles, the high number of donor atoms between 7 and 10, and the dinuclear composition obtained in all the systems examined, point out that in the formed solid complexes both Ca2+ ions could be located inside of the macrocycle cavities. Transmetallation reaction of a lanthanide(III) complex, [L5Sm](ClO4)3·9H2O, with Ca(ClO4)2·xH2O leads the formation of the new dinuclear orange [L5Ca2](ClO4)4·3H2O complex, manifesting the versatility of this macrocyclic cavity. All complexes have been characterized by microanalysis, IR, UV‐vis, 1H NMR spectroscopy, FAB mass spectrometry, FAAS spectroscopy, and conductivity measurements. 相似文献
8.
The coordination capability of two pendant-armed azamacrocyclic ligands with cyanoethyl L1and cyanomethyl L2 pendant groups towards cadmium nitrate and perchlorate salts was achieved. All metal complexes were characterized by elemental analysis, LSI-MS, IR, conductivity measurements and 1H NMR spectroscopy. The X-ray crystal structure of the complexes [CdL1](NO3)2, [CdL1](ClO4)2 · CH3CN, and [CdL2](ClO4)2 · H2O were also determined. All the complexes are mononuclear with the metal ion in a distorted octahedral environment. The pendant groups are not coordinated to the metal due the linear nature of the cyano groups; however, different interactions between nitrate ions, nitrile groups and pyridine rings from the macrocycle have been observed in the Cd(II) complexes with L1. 相似文献
9.
Unprecedented 1D Mixed-metal Polynuclear Cyclometalated Platinum Complexes: Synthesis, Structural Characterization and Spectroscopic Properties 总被引:1,自引:0,他引:1
The complexes [Pt2L2(μ-dppm)](ClO4)2 (1) and {[Pt2L2(μ-dppm)Li(CH3CN)2](ClO4)3}n (2), where HL is 6-[4-(diethoxyphosphorylmethyl)phenyl]-2,2′-bipyridinyl and dppm is bis(diphenylphosphino)methane, have been synthesized and characterized. In complex 1 the platinum(Ⅱ) center adopts a distorted square planar coordination geometry. The polymer 2 exhibits a "stairstep" configuration with one-dimensional Pt(Ⅱ)N^N^CPO- Li(Ⅰ)-OPC^N^ NPt(Ⅱ) mixed-metal units which are linked through dppm. Both complexes have metal-metal interaction with Pt- Pt distances of 3.325(2) and 3.1432(9) A, respectively, and display strong metal-metal-to-ligand charge-transfer (MMLCT) triplet state emission. The density-functional-theory calculation was used to interpret the absorption spectra of the complexes. 相似文献
10.
《Acta Crystallographica. Section C, Structural Chemistry》2018,74(8):961-966
The self‐assembly of metal–polydentate ligands to give supramolecular tetrahedral complexes is of considerable current interest. A new ligand, 4‐benzyl‐2‐[1‐(2‐{[3‐(4‐benzylpyridin‐2‐yl)‐1H‐pyrazol‐1‐yl]methyl}benzyl)‐1H‐pyrazol‐3‐yl]pyridine (L), with chelating pyrazolyl–pyridine units substituted on the 4‐position of the pyridyl ring with benzyl units, has been synthesized and fully characterized. The self‐assembly of L with cobalt(II) gave rise to a tetrahedral cage (hexakis{μ‐4‐benzyl‐2‐[1‐(2‐{[3‐(4‐benzylpyridin‐2‐yl)‐1H‐pyrazol‐1‐yl]methyl}benzyl)‐1H‐pyrazol‐3‐yl]pyridine}perchloratotetracobalt(II) octakis(perchlorate) acetonitrile undecasolvate, [Co4(ClO4)(C38H32N6)6](ClO4)7·11CH3CN) with approximate T symmetry. The X‐ray crystal structure of the cage, i.e. [Co4L6ClO4](ClO4)7, shows that the substituted benzyl groups are oriented away from the centres of their respective ligands towards the CoII vertices, making small outward‐facing pockets from three benzyl rings at the corners of the tetrahedron. 相似文献
11.
The reactions of different nickel(II) salts with a mixed‐donor macrocyclic ligand L (6,7,8,9,10,11,18,19‐octahydro‐5H, 17H‐dibenzo[f,o][1,5,9,13] dioxadiazacyclohexadecin‐18‐ol), potentially pentadentate N2O3 donor sets containing one pendant alcohol function have been investigated. The physical properties and the chemical structures of 1:1 (metal:ligand) NiLX2 (X = Cl?, Br?, NO3?, ClO4?) complexes have been characterized by using IR, UV‐Vis spectroscopy and conductance measurements. The X‐ray determination have been employed to probe the nature of the respective complexes in solid state. The nickel atom in [NiL(NO3)]NO3·0.5H2O complex is six‐coordinate with a distorted octahedral coordination in which the all N2O3 donor atoms are coordinated to the nickel atom. The coordination sphere is completed by a nitrate anion. In contrast to the above nickel complex, in [NiLCl2] complex the pendant hydroxyl arm of macrocycle remains uncoordinated and ligand acts as tetradentate N2O2 donor atoms. The coordination sphere is completed by two chloride anions and the nickel atom is six‐coordinate with a distorted octahedral coordination. 相似文献
12.
Jing Xie Yong‐Qing Huang Taka‐aki Okamura Wei‐Yin Sun Prof. Dr. Norikazu Ueyama 《无机化学与普通化学杂志》2007,633(8):1211-1216
Reactions of new unsymmetrical pyridyl‐ and imidazoyl‐containing tripodal ligand, 3‐(1H‐imidazol‐1‐yl)‐N,N‐bis(2‐pyridylmethyl)propan‐1‐amine ( L ), with varied silver(I) salts result in formation of three supramolecular architectures [Ag2L2](BF4)2·H2O ( 1 ), [Ag2L2](ClO4)2·H2O ( 2 ) and [Ag3L2](CF3SO3)3 ( 3 ). All the structures were established by single‐crystal X‐ray diffraction analysis. In the solid state, three complexes consist of one‐dimensional infinite chains, in which the conformation and the bridging mode of L for complexes 1 and 2 are the same but 3 different. There are Ag···Ag and π‐π interactions in 3 . The results imply that the shape and size of the anion have great impact on the structure of the complexes. The complexes were also characterized by electrospray mass spectrometry. 相似文献
13.
The new synthesized ligand (DADMBTZ = 2,2′‐diamino‐5,5′‐dimethyl‐4,4′‐bithiazole), which is mentioned in this text, is used for preparing the two new complexes [Zn(DADMBTZ)3](ClO4)2. 0.8MeOH.0.2H2O ( 1 ) and [Cd(DADMBTZ)3](ClO4)2 ( 2 ). The characterization was done by IR, 1H, 13C NMR spectroscopy, elemental analysis and single crystal X‐ray determination. In reaction with DADMBTZ, zinc(II) and cadmium(II) show different characterization. In 2 , to form a tris‐chelate complex with nearly C3 symmetry for coordination polyhedron, DADMBTZ acts as a bidentate ligand. In 1 , this difference maybe relevant to small radii of Zn2+ which make one of the DADMBTZ ligands act as a monodentate ligand to form the five coordinated Zn2+ complex. In both 1 and 2 complexes the anions are symmetrically different. 1 and 2 complexes form 2‐D and 3‐D networks via N‐H···O and N‐H···N hydrogen bonds, respectively. 相似文献
14.
《Journal of Coordination Chemistry》2012,65(5):910-920
Two new dinuclear macrocyclic complexes, [Ni2L1(OAc)]·ClO4 (1) and [Co2L2(OAc)]·1.5(ClO4)·0.5Na·2(CH3OH) (2) (where H2L1 and H2L2 are the condensation products of N,N-bis(3-aminopropyl)-4-methoxybenzylamine with 2,6-diformyl-4-brominephenol and 2,6-diformyl-4-methylphenol in the presence of metal ions, respectively) have been synthesized and characterized by infrared spectra, elemental analysis, electrospray mass spectra, and X-ray single crystal diffraction. The interactions of the complexes with CT-DNA have been measured by UV-absorption titrations and fluorescence quenching experiments. 相似文献
15.
以三氨乙基胺和N-甲基咪唑醛为原料合成了三角架多咪唑配体((min)3tren),并合成了五个过渡金属配合物:[Zn(min)3tren](ClO4)21, [Cu(min)3tren](ClO4)22, [Ni(min)3tren](ClO4)23, [Co(min)3tren](ClO4)24, and [Mn(min)3tren](ClO4)2CH3CN
5,通过元素分析,摩尔电导率,红外和电子光谱确定了化合物的组成。对配合物4和5进行了晶体结构测定。结果表明,在这两个化合物中金属原子均处于扭曲的八面体配位环境,分别与三个亚胺氮原子和三个咪唑氮原子配位。配合物4和5的电化学研究表明在乙腈溶液中,有[Co-O2]n-和[Mn-O2]n-存在,认为4和5是很好的超氧化物清除剂。 相似文献
16.
The N‐functionalized macrocyclic ligand 2,13‐bis(1‐naphthalenylmethyl)‐5,16‐dimethyl‐2,6,13,17‐tetraazatricyclo(14,4,01.18,07.12)docosane (L3) and its copper(II) complex were prepared. The crystal structure of [Cu(L3)](ClO4)2·2CH3CN was determined by single‐crystal X‐ray diffraction at 150 K. The copper atom, which lies on an inversion centre, has a square planar arrangement and the complex adopts a stable trans‐III configuration. The longer distance [2.081(2) Å] for Cu–N(tertiary) compared to 2.030(3) Å for Cu–N(secondary) may be due to the steric effect of the attached naphthalenylmethyl group on the tertiary nitrogen atom. Two perchlorate ions are weakly attached to copper in axial sites and are further connected to the ligand of the cation through NH ··· O hydrogen bonds [N ··· O 3.098 Å]. IR and UV/Vis spectroscopic properties are also described. 相似文献
17.
Two novel five‐coordinate zinc(II) complexes with the tripod ligand tris(N‐methylbenzimidazol‐2‐ylmethyl)amine (Mentb) and two different α,β‐unsaturated carboxylates, with the composition [Zn(Mentb)(acrylate)] (ClO4)·DMF·1.5CH3OH ( 1 ) and [Zn(Mentb)(cinnamate)](ClO4)·2DMF·0.5CH3OH ( 2 ), were synthesized and characterized by means of elemental analyses, electrical conductivity measurements, IR, UV, and 1H NMR spectra. The crystal structure of two complexes have been determined by a single‐crystal X‐ray diffraction method, and show that the ZnII atom is bonded to a Mentb ligand and a α,β‐unsaturated carboxylate molecule through four N atoms and one O atom, resulting in a distorted trigonal‐bipyramidal coordination [τ( 1 ) = 0.853, τ( 2 ) = 0.855], with approximate C3 symmetry. 相似文献
18.
Spontaneous Reduction of Mononuclear High‐Spin Iron(III) Complexes to Mononuclear Low‐Spin Iron(II) Complexes in Aqueous Media and Nuclease Activity via Self‐Activation
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Mononuclear high‐spin [FeIII(Pyimpy)Cl3]?2 CH2Cl2 ( 1 ?2 CH2Cl2) and [FeIII(Me‐Pyimpy)Cl3] ( 2 ), as well as low‐spin FeII(Pyimpy)2](ClO4)2 ( 3 ) and [FeII(Me‐Pyimpy)2](ClO4)2 ( 4 ) complexes of tridentate ligands Pyimpy and Me‐Pyimpy have been synthesized and characterized by analytical techniques, spectral, and X‐ray structural analyses. We observed an important type of conversion and associated spontaneous reduction of mono‐chelated high‐spin FeIII ( 1 ?2 CH2Cl2 and 2 ) complexes to low‐spin bis‐chelated FeII complexes 3 and 4 , respectively. This process has been explored in detail by UV/Vis, fluorescence, and 1H NMR spectroscopic measurements. The high positive potentials observed in electrochemical studies suggested a better stabilization of FeII centers in 3 and 4 . Theoretical studies by density functional theory (DFT) calculations supported an increased stabilization for 3 in polar solvents. Self‐activated nuclease activity of complexes 1 ?2CH2Cl2 and 2 during their spontaneous reduction was examined for the first time and the mechanism of nuclease activity was investigated. 相似文献
19.
Regioselective Synthesis and Characterization of Multinuclear Convex‐Bound Ruthenium‐[n]Cycloparaphenylene (n=5 and 6) Complexes
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Dr. Eiichi Kayahara Dr. Vijay Kumar Patel Audrey Mercier Prof. Dr. E. Peter Kündig Prof. Dr. Shigeru Yamago 《Angewandte Chemie (International ed. in English)》2016,55(1):302-306
Mono‐ and multinuclear complexes of ruthenium and [n]cycloparaphenylene (CPP, n=5 and 6) were synthesized in excellent yields through ligand exchange of the cationic complex [(Cp)Ru(CH3CN)3](PF6) with CPP. In the multinuclear complexes, ruthenium selectively coordinated to alternate paraphenylene units to give bis‐ and tris‐coordinated Ru complexes for [5] and [6]CPPs, respectively. Single‐crystal X‐ray analysis revealed the Ru was coordinated with η6‐hapticity on the convex surface of CPP. 相似文献
20.
Jiliang Wang Hongfeng Li Peng Chen Meiqi Zhang Wenbin Sun Pengfei Yan 《无机化学与普通化学杂志》2016,642(5):368-371
The reaction of 2‐aldehyde‐8‐hydroxyquinoline, histamine, and YbX3 · 6H2O (X = NO3–, ClO4–) affords two ytterbium complexes [Yb(nma)2] · ClO4 · 2CH2Cl2 ( 1 ) and [Yb(nma)(NO3)2(DMSO)] · CH3OH ( 2 ) (Hnma = N‐(2‐(8‐hydroxylquinolinyl)methane(2‐(4‐imidazolyl)ethanamine))). The crystal structures were determined by X‐ray diffraction and it has been revealed that the anions have played important role in the assembly. In the case of 1 , the Yb3+ ions are completely encapsulated by two nma ligands with uncoordinated perchlorate anion balancing the positive charge. In the case of 2 , the Yb3+ ions are ligated by the ligand, oxygen atoms of the nitrate ion, and DMSO. Both complexes exhibit essential NIR luminescence of Yb3+ ions. 相似文献