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1.
Rituparna Biswas Yumi Ida Dr. Michael L. Baker Saptarshi Biswas Paramita Kar Prof. Dr. Hiroyuki Nojiri Prof. Dr. Takayuki Ishida Prof. Dr. Ashutosh Ghosh 《Chemistry (Weinheim an der Bergstrasse, Germany)》2013,19(12):3943-3953
Three new trinuclear nickel (II) complexes with the general composition [Ni3L3(OH)(X)](ClO4) have been prepared in which X=Cl? ( 1 ), OCN? ( 2 ), or N3? ( 3 ) and HL is the tridentate N,N,O donor Schiff base ligand 2‐[(3‐dimethylaminopropylimino)methyl]phenol. Single‐crystal structural analyses revealed that all three complexes have a similar Ni3 core motif with three different types of bridging, namely phenoxido (μ2 and μ3), hydroxido (μ3), and μ2‐Cl ( 1 ), μ1,1‐NCO ( 2 ), or μ1,1‐N3 ( 3 ). The nickel(II) ions adopt a compressed octahedron geometry. Single‐crystal magnetization measurements on complex 1 revealed that the pseudo‐three‐fold axis of Ni3 corresponds to a magnetic easy axis, being consistent with the magnetic anisotropy expected from the coordination structure of each nickel ion. Temperature‐dependent magnetic measurements indicated ferromagnetic coupling leading to an S=3 ground state with 2J/k=17, 17, and 28 K for 1 , 2 , and 3 , respectively, with the nickel atoms in an approximate equilateral triangle. The high‐frequency EPR spectra in combination with spin Hamiltonian simulations that include zero‐field splitting parameters DNi/k=?5, ?4, and ?4 K for 1 , 2 , and 3 , respectively, reproduced the EPR spectra well after a anisotropic exchange term was introduced. Anisotropic exchange was identified as Di,j/k=?0.9, ?0.8, and ?0.8 K for 1 , 2 , and 3 , respectively, whereas no evidence of single‐ion rhombic anisotropy was observed spectroscopically. Slow relaxation of the magnetization at low temperatures is evident from the frequency‐dependence of the out‐of‐phase ac susceptibilities. Pulsed‐field magnetization recorded at 0.5 K shows clear steps in the hysteresis loop at 0.5–1 T, which has been assigned to quantum tunneling, and is characteristic of single‐molecule magnets. 相似文献
2.
Poly[[μ2‐aqua‐bis[(1,10‐phenanthroline)nickel(II)]]‐di‐μ2,μ4‐5‐nitro‐1,3‐benzenedicarboxylato]
Hong‐Yin He Yi‐Li Zhou Long‐Guan Zhu 《Acta Crystallographica. Section C, Structural Chemistry》2004,60(11):m569-m571
The reaction of Ni(CH3COO)2·4H2O, 5‐nitro‐1,3‐benzenedicarboxylic acid (H2nmbdc), 1,10‐phenanthroline and water under hydrothermal conditions yields the first reported two‐dimensional nickel coordination polymer with water‐ and carboxylate‐bridged dimeric units, viz. [Ni2(C8H3NO6)2(C12H8N2)2(H2O)]n. The coordination polyhedron of the NiII ion in the title structure is an octahedron defined by an N2O4 donor set. The water molecule is positioned on a mirror plane and the 5‐nitro‐1,3‐benzenedicarboxylate group is located on a twofold axis. Two types of nmbdc2− coordination mode are observed: one is a bis‐monodentate mode, μ2‐nmbdc2−, and the other is a bis‐bridging mode, μ4‐nmbdc2−. The dimeric unit in the title compound is similar to the structural moiety in urease. In the two‐dimensional framework in the title compound, strong stacking interactions between benzene rings (μ2‐nmbdc2− and μ4‐nmbdc2−) and 1,10‐phenanthroline ligands are observed. 相似文献
3.
Esteban J Ruiz E Font-Bardia M Calvet T Escuer A 《Chemistry (Weinheim an der Bergstrasse, Germany)》2012,18(12):3637-3648
A series of nickel complexes with nuclearity ranging from Ni(3) to Ni(6) have been obtained by treatment of a variety of nickel salts with the 2-pyridylcyanoxime ligand. The reported compounds have as a common structural feature the triangular arrangement of nickel cations bridged by a central μ(3)-oxo/alkoxo ligand. These compounds are simultaneously the first nickel derivatives of the 2-pyridylcyanoxime ligand and the first examples of isolated, μ(3)-O triangular pyridyloximate nickel complexes. Magnetic measurements reveal antiferromagnetic interactions promoted by the μ(3)-O and oximato superexchange pathways and comparison of the experimental structural and magnetic data with DFT calculations give an in-depth explanation of the factors that determine the magnetic interaction in this kind of system. 相似文献
4.
Gansheng Huang Dongsheng Liu Xihe Huang Changcang Huang Xiaohuan Qin 《Acta Crystallographica. Section C, Structural Chemistry》2008,64(11):m369-m371
In the title compound, [Pb(C6H4NO2)(N3)(H2O)]n, the Pb ion is seven‐coordinated by three N atoms from three azide ligands, two O atoms from two isonicotinate (inic) ligands and two O atoms from two coordinated water molecules, forming a distorted monocapped triangular prismatic coordination geometry. Each azide ligand bridges three PbII ions in a μ1,1,3 coordination mode to form a two‐dimensional three‐connected 63 topology network extending in the bc plane. The carboxylate group of the inic unit and the aqua ligand act as coligands to bridge PbII ions. Adjacent two‐dimensional layers are connected by hydrogen‐bonding interactions between the isonicotinate N atom and the water molecule, resulting in an extended three‐dimensional network. The title complex is the first reported coordination polymer involving a p‐block metal, an azide and a carboxylate. 相似文献
5.
Azizolla Beheshti William Clegg Sophie H. Dale Reza Hyvadi 《Acta Crystallographica. Section C, Structural Chemistry》2009,65(8):m314-m316
The title complex, [Zn(C15H22BN6)(C2H3O2)] or (TpMe,Me)Zn(OAc), contains a tripodal tris(pyrazolyl)hydroborate ligand, a monodentate acetate ligand and a ZnII centre in a distorted tetrahedral coordination environment capped on one triangular face by a secondary Zn...O interaction with the second O atom of the acetate ligand. The four‐coordination of ZnII and the essentially monodentate character of the acetate ligand are due to the high steric demands of the ligand set, which prevent chelate formation and five‐coordination and lead to relatively long Zn—O and Zn—N bonds compared with related complexes of ZnII and other metals. 相似文献
6.
A. Castieiras M. C. F. Vidal J. Romero R. Sez A. Matilla J. Nicls J. M. Tercero 《无机化学与普通化学杂志》2001,627(7):1553-1559
New dinuclear complexes of the types [Ni2(L)(H2O)2] and [Ni2(L)(H2O)6] [H4L = N,N′‐bis(carboxymethyl) dithiooxamide (H4GLYDTO), N,N′‐bis(1‐carboxyethyl) dithiooxamide (H4ALADTO), N,N′‐bis(1‐carboxy‐2‐methylpropyl) dithiooxamide (H4VALDTO) and N,N′‐bis(1‐carboxy‐3‐methylbutyl) dithiooxamide (H4LEUDTO)] have been prepared and characterized by IR and electronic absorption spectroscopy, and the structure of [Ni2(ALADTO)(H2O)6] crystals has been determined by single crystal X‐ray analysis. This compound is composed of discrete dinuclear units in which two NiII atoms with NO4S kernels are linked by a single [ALADTO]4– group that coordinates through its carboxylato oxygen, amino nitrogen and thiolato sulphur atoms. In each dimer unit the two nickel(II) ions in distorted octahedral coordination are separated by 5.863(2) Å The temperature dependence of the magnetic susceptibility of the new compounds was measured over the range 2 to 300 K. In the complexes of [GLYDTO]4– and [ALADTO]4– the two Ni atoms are antiferromagnetically coupled, with J = –23.51(4) and –20.95(8) cm–1, respectively. By constrast, [Ni2(VALDTO)(H2O)2], [Ni2(VALDTO)(H2O)6] and [Ni2(LEUDTO)(H2O)2] remain paramagnetic down to 2 K, with magnetic moment values between 2.8 and 3.3 M.B. 相似文献
7.
A three‐dimensional polymeric NiII complex, [Ni(bpp)(NIP)(H2O)]n (bpp = 1,3‐di(4‐pyridyl)propane and NIP = 5‐nitroisophthalate), has been synthesized and characterized. The coordination number of the nickel atom is six (NiN2O4) and the coordination environment around the NiII atom may be described as a distorted octahedron in which two nitrogen atoms of “bpp” ligand occupy the cis positions. The effective magnetic moment for this complex indicate that the interactions between two NiII atoms through the effective exchange media are antiferromagnetic. Self‐assembly of these compounds in the solid state via π–π‐stacking interactions is discussed. 相似文献
8.
Bin Liu Jing‐Wen Chen Xiao‐Qing Chen Yi‐Zhi Li 《Acta Crystallographica. Section C, Structural Chemistry》2007,63(2):m42-m44
The asymmetric unit of the title compound, [Ni2(C25H31N4O3)(C2H3O2)2]PF6·0.5H2O, consists of two dinuclear nickel cations, two hexafluorophosphate anions and one water molecule of crystallization. Within each cation, the Ni atoms are bridged by two exogenous acetate groups and an endogenous cresol O atom of a phenolate‐based `end‐off' compartmental ligand that possesses two pendant chelating arms attached to the ortho positions of the phenol ring. Each Ni atom is six‐coordinate with a slightly distorted octahedral geometry. The two symmetry‐independent cations are linked into a dimeric unit through O—H⋯O hydrogen bonds. Additional O—H⋯O, C—H⋯F and C—H⋯O intermolecular interactions link all of the units in the structure into a three‐dimensional framework. 相似文献
9.
Cengiz Arici Filiz Ercan Raif Kurtaran Orhan Atakol 《Acta Crystallographica. Section C, Structural Chemistry》2001,57(7):812-814
In the title compounds, {2,2′‐[2,2‐dimethyl‐1,3‐propanediylbis(nitrilomethylidyne)]diphenolato‐κ4N,N′,O,O′}nickel(II), [Ni(C19H20N2O2)], and {2,2′‐[2,2‐dimethyl‐1,3‐propanediylbis(nitrilomethylidyne)]diphenolato‐κ4N,N′,O,O′}copper(II), [Cu(C19H20N2O2)], the NiII and CuII atoms are coordinated by two iminic N and two phenolic O atoms of the N,N′‐bis(salicylidene)‐2,2‐dimethyl‐1,3‐propanediaminate (SALPD2?, C17H16N2O22?) ligand. The geometry of the coordination sphere is planar in the case of the NiII complex and distorted towards tetrahedral for the CuII complex. Both complexes have a cis configuration imposed by the chelate ligand. The dihedral angles between the N/Ni/O and N/Cu/O coordination planes are 17.20 (6) and 35.13 (7)°, respectively. 相似文献
10.
Pseudohalide‐directed Assembly of Two Zinc(II) Coordination Polymers with a 3,4‐Bis(3‐pyridyl)‐5‐(4‐pyridyl)‐1,2,4‐triazole Tecton
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The zinc(II) pseudohalide complexes {[Zn(L334)(SCN)2(H2O)](H2O)2}n ( 1 ) and [Zn(L334)(dca)2]n ( 2 ) were synthesized and characterized using the ligand 3,4‐bis(3‐pyridyl)‐5‐(4‐pyridyl)‐1,2,4‐triazole (L334) and ZnCl2 in presence of thiocyanate (SCN–) and dicynamide [dca, N(CN)2–] respectively. Single‐crystal X‐ray structural analysis revealed that the central ZnII atoms in both complexes have similar octahedral arrangement. Compound 1 has a 2D sheet structure bridged by bidentate L334 and double μN,S‐thiocyanate anions, whereas complex 2 , incorporating with two monodentate dicynamide anions, displays a two‐dimensional coordination framework bridged by tetradentate L334 ligand. Structural analysis demonstrated that the influence of pseudohalide anions plays an important role in determining the resultant structure. Both complexes were characterized by IR spectroscopy, microanalysis, and powder X‐ray diffraction techniques. In addition, the solid fluorescence and thermal stability properties of both complexes were investigated. 相似文献
11.
Abdulnasir A. Majeed Mostafa M.H. Khalil Ahmed Fetoh Ayman A. Abdel Aziz G.M. Abu El‐Reash 《应用有机金属化学》2021,35(1)
In this work, (Z)‐N‐benzoyl‐N′‐(1H‐1,2,4‐triazol‐3‐yl)carbamimidothioic acid and its Mn(II), Co(II), Cu(II) and Cd(II) complexes were introduced for the first time. This carbonyl thiourea ligand was prepared by the reaction of 1H‐1,2,4‐triazol‐3‐amine with benzoyl isothiocyanate. The structural elucidation of these compounds was performed using elemental analysis and spectral and magnetic measurements. Octahedral structures of all complexes, except Cd(II) complex with a tetrahedral geometry, were confirmed by applying DFT structural optimization. The thermal decomposition behaviour of metal complexes of carbonyl thiourea ligand is discussed. The calculation of kinetic parameters for prepared complexes (Ea, A, ΔH*, ΔS* and ΔG*) of all thermal degradation stages has been evaluated using two comparable approaches. Antimicrobial and ABTS‐antioxidant studies indicated potent activity of Cd(II) complex compared with the other investigated compounds. The cytotoxic activity of the prepared compounds was investigated in vitro. The results indicated potent activity of Mn(II) complex against both HePG2 (liver carcinoma) and MCF‐7 (breast carcinoma) cancer cells. 相似文献
12.
Yi Ma Li‐Tian Zhang Xiao‐Fang Wang Yong‐Ke He Zheng‐Bo Han 《Acta Crystallographica. Section C, Structural Chemistry》2007,63(12):m573-m575
A new coordination polymer, catena‐poly[[(dipyrido[3,2‐a:2′,3′‐c]phenazine‐κ2N,N′)nickel(II)]‐μ‐2,6‐dipicolinato‐κ4O2,N,O6:O2′], [Ni(C7H3NO4)(C18H10N4)]n, exhibits a one‐dimensional structure in which 2,6‐dipicolinate acts as a bridging ligand interconnecting adjacent nickel(II) centers to form a chain structure. The asymmetric unit contains one NiII center, one dipyrido[3,2‐a:2′,3′‐c]phenazine ligand and one 2,6‐dipicolinate ligand. Each NiII center is six‐coordinated and surrounded by three N atoms and three O atoms from one dipyrido[3,2‐a:2′,3′‐c]phenazine ligand and two different 2,6‐dipicolinate ligands, leading to a distorted octahedral geometry. Adjacent chains are linked by π–π stacking interactions and weak interactions to form a three‐dimensional supramolecular network. 相似文献
13.
14.
Mikhail M. Degtyarik Alexander S. Lyakhov Ludmila S. Ivashkevich Dr. Sergei V. Voitekhovich Gennady T. Sukhanov Yuri V. Grigoriev 《无机化学与普通化学杂志》2012,638(6):950-956
1‐(2‐Hydroxyethyl)‐3‐nitro‐1, 2, 4‐triazole (hnt), prepared by alkylation of 3‐nitro‐1, 2, 4‐triazole with 2‐chloroethanol, was found to react with copper(II) chloride and copper(II) perchlorate in acetonitrile/ethanol solutions giving complexes [Cu2(hnt)2Cl4(H2O)2] and[Cu(hnt)2(H2O)3](ClO4)2, respectively. They are the first examples of coordination compounds with a neutral N‐substituted 3‐nitro‐1, 2, 4‐triazole ligand. 1‐(2‐Hydroxyethyl)‐3‐nitro‐1, 2, 4‐triazole and the obtained complexes were characterized by NMR and IR spectroscopy, X‐ray, and thermal analyses. [Cu2(hnt)2Cl4(H2O)2] presents a dinuclear chlorido‐bridged complex in which hnt acts as a chelating bidentate ligand, coordinated to the metal by a nitrogen atom of the triazole ring and an oxygen atom of the nitro group, and the copper atoms are inconsiderably distorted octahedral coordination. [Cu(hnt)2(H2O)3](ClO4)2comprises a mononuclear complex cation, in which two nitrogen atoms of two hnt ligands in trans configuration and three water oxygen atoms form a square pyramidal environment around the copper atom, which is completed to an distorted octahedron with a bifurcated vertex due to two additional elongated Cu–O bonds with two nitro groups. In both complexes, Cu–O bonds with the nitro groups may be considered as semi‐coordinated. 相似文献
15.
Man‐Sheng Chen Jin‐Sheng Xu Yi‐Fang Deng Chun‐Hua Zhang 《Acta Crystallographica. Section C, Structural Chemistry》2013,69(10):1124-1127
In the title compound, [Ni(C14H8N2O5)(H2O)2]n, the NiII cation is six‐coordinate with a slightly distorted octahedral coordination geometry and the 4‐(isonicotinamido)phthalate ligand links the NiII centres into a three‐dimensional structure with sra topology. The structure is also stabilized by N—H...O hydrogen bonding between the uncoordinated amide groups of the ligand and extensive O—H...O hydrogen bonding between the two coordinated water molecules. The magnetic and thermal stability properties of the title compound are also discussed. 相似文献
16.
A series of new 3‐(arylhydrazono)pentane‐2, 4‐diones ( 1 ‐ 6 ) synthesized from pentane‐2, 4‐dione and diazonium salts of respective anilines using the procedure of Japp‐Klingemann are described. Complexes with CuII and NiII salts are prepared ( 7 ‐ 10 , respectively). Spectroscopic properties of these compounds have been studied and X‐ray crystal structures of selected hydrazones ( 3 , 4 , 6 ) and of the hydrazone complexes ( 7 ‐ 10 ) are reported. The structures of the uncomplexed hydrazones feature an intramolecular N‐H···O interaction to yield a six‐membered H‐bond ring reflecting preference of the hydrazone tautomeric structure. All the complexes are mononuclear 2:1 (L:M) structures of six‐membered chelate type involving N2O2 binding sites that are quadratic arranged but differ in the entire coordination environment dependent on the metal and the ligand substitution including distorted octahedral and quadratic pyramidal coordination geometries in the CuII complexes 7 and 8 or nearly regular square planar coordination geometry in the NiII complexes 9 and 10 , respectively. In the crystal packings, strong and weak H‐bond interactions cause supramolecular network structures. 相似文献
17.
Tomoka Yamaguchi Yukinari Sunatsuki Hiroyuki Ishida 《Acta Crystallographica. Section C, Structural Chemistry》2008,64(4):m156-m160
In the crystal structures of both title compounds, [1,3‐bis(2‐hydroxybenzylidene)‐2‐methyl‐2‐(2‐oxidobenzylideneaminomethyl)propane‐1,3‐diamine]nickel(II) [2‐(2‐hydroxybenzylideneaminomethyl)‐2‐methyl‐1,3‐bis(2‐oxidobenzylidene)propane‐1,3‐diamine]nickel(II) chloride methanol disolvate, [Ni(C26H25.5N3O3)]2Cl·2CH4O, and [1,3‐bis(2‐hydroxybenzylidene)‐2‐methyl‐2‐(2‐oxidobenzylideneaminomethyl)propane‐1,3‐diamine]zinc(II) perchlorate [2‐(2‐hydroxybenzylideneaminomethyl)‐2‐methyl‐1,3‐bis(2‐oxidobenzylidene)propane‐1,3‐diamine]zinc(II) methanol trisolvate, [Zn(C26H25N3O3)]ClO4·[Zn(C26H26N3O3)]·3CH4O, the 3d metal ion is in an approximately octahedral environment composed of three facially coordinated imine N atoms and three phenol O atoms. The two mononuclear units are linked by three phenol–phenolate O—H...O hydrogen bonds to form a dimeric structure. In the Ni compound, the asymmetric unit consists of one mononuclear unit, one‐half of a chloride anion and a methanol solvent molecule. In the O—H...O hydrogen bonds, two H atoms are located near the centre of O...O and one H atom is disordered over two positions. The NiII compound is thus formulated as [Ni(H1.5L)]2Cl·2CH3OH [H3L is 1,3‐bis(2‐hydroxybenzylidene)‐2‐(2‐hydroxybenzylideneaminomethyl)‐2‐methylpropane‐1,3‐diamine]. In the analogous ZnII compound, the asymmetric unit consists of two crystallographically independent mononuclear units, one perchlorate anion and three methanol solvent molecules. The mode of hydrogen bonding connecting the two mononuclear units is slightly different, and the formula can be written as [Zn(H2L)]ClO4·[Zn(HL)]·3CH3OH. In both compounds, each mononuclear unit is chiral with either a Δ or a Λ configuration because of the screw coordination arrangement of the achiral tripodal ligand around the 3d metal ion. In the dimeric structure, molecules with Δ–Δ and Λ–Λ pairs co‐exist in the crystal structure to form a racemic crystal. A notable difference is observed between the M—O(phenol) and M—O(phenolate) bond lengths, the former being longer than the latter. In addition, as the ionic radius of the metal ion decreases, the M—O and M—N bond distances decrease. 相似文献
18.
Sergio Baggio M. Enriqueta Díaz de Vivar Ricardo Baggio María Teresa Garland 《Acta Crystallographica. Section C, Structural Chemistry》2006,62(5):m195-m198
The title compound, [Cd2(SO3)2(C18H12N6)2]·8H2O, is a dimer built up around a symmetry center, where the sulfite anion displays a so far unreported coordination mode in metal‐organic complexes; the anion binds as a μ2‐sulfite‐κ4O,O′:O′,O′′ ligand to two symmetry‐related seven‐coordinate CdII cations, binding through its three O atoms by way of two chelate bites with an O atom in common, which acts as a bridge. The cation coordination is completed by a 2,4,6‐tri‐2‐pyridyl‐1,3,5‐triazine ligand acting in its usual tridentate mode. 相似文献
19.
Guo‐Wu Lin Yue Wang Tao Lu 《Acta Crystallographica. Section C, Structural Chemistry》2008,64(4):m179-m181
The title compound, [Co(C19H15N3O5S)(C12H8N2)]·5H2O, has a moderately distorted octahedral coordination environment composed of two N atoms of a 1,10‐phenanthroline ligand and one N and three O atoms of an N‐{[4‐(1,3‐benzothiazol‐2‐yl)anilino]carbonylmethyl}iminodiacetate (ZL‐52−) ligand. The ring systems of the phenanthroline and ZL‐52− ligands are coplanar and the complexes pack in layers parallel to the ab plane with the rings of adjacent complexes facing one another. The layers stack along the c axis and are linked by hydrogen bonds involving the five water solvent molecules in the asymmetric unit and O atoms of the acetate groups of the ZL‐52− ligand. This is believed to be the first crystal structure of a complex of a 2‐(4‐aminophenyl)benzothiazole ligand. 相似文献
20.
A new polymorph of a mononuclear nickel(II) acetate complex with 2‐(pyridin‐2‐yl)ethanol ligands, [Ni(CH3COO)2(C7H9NO)2], has been prepared and structurally characterized. Its molecular structure resembles the structures of two previously reported polymorphs in that the NiII atom is located on an inversion centre and is coordinated by pairs of acetate and 2‐(pyridin‐2‐yl)ethanol ligands. The acetate anions are coordinated in a monodentate manner, while the 2‐(pyridin‐2‐yl)ethanol ligands are coordinated in a bidentate chelating mode involving the endocyclic N atom and the hydroxy O atom of the ligand side chain. A strong bifurcated intramolecular hydrogen‐bond interaction was observed involving the hydroxy O atom as donor and both acetate O atoms as acceptors. No classical intermolecular hydrogen‐bond contacts were observed. However, the crystal packing is effected through π–π and C—H...π interactions, giving rise to a different packing arrangement. A brief comparison of the three polymorphic forms is presented. 相似文献