Preparation and X-Ray crystal structure of a Novel Nickel(II) complex with dithiocarbimate

The reaction of potassiumN-(methanesulfonyl)-dithiocarbimate, K₂[S₂C=NSO₂CH₃], with nickel(II) chloride hexahydrate, NiCl₂·6H₂O, formed the complex anion bis(N-(methanesulfonyl)-dithiocarbimate)nickelate(II), [Ni(S₂C=NSO₂CH₃)₂]^2}-, which was isolated as its tetra-n-butylammonium salt. The UV-Vis data obtained were consistent with the formation of a nickelsulfur diamagnetic planar complex. The¹H NMR and the¹³C NMR spectra showed the expected signals for then-Bu₄N⁺ cation and the dithiocarbimate moiety. The single-crystal structure analysis showed that tetra-n-butylammonium bis(N-(methanesulfonyl)-dithiocarbimate)nickelate(II), (Bu₄N)₂[Ni(S₂C=NSO₂CH₃)₂], crystallizes in the monoclinic space groupP2_l/c witha=9.3197(5),b=15.0795(8),c=17.5286(9) å,=91.262(3),V=2462.8(3) å³, andZ=2. The nickel atom is coordinated to four sulfur atoms.     

一个不常见的Ni(Ⅱ)的戊三酮二水杨酰腙配合物的合成和晶体结构

合成了镍的戊三酮二水杨酰腙配合物Ni(C₁₉H₁₆N₄O₅)的两个同质异晶,测定其晶体结构。该配合物的两个晶体均属单斜晶系,空间群为C2/c,晶体1晶胞参数为:a=1.03076(9)nm,b=1.9105(1)nm,c=0.93305(8)nm,β=101.490(4)°,Z=4,μ=1.119mm^-1,R=0.0370;晶体2晶胞参数为:a=2.1949(3)nm,b=0.9901(2)nm,c=0.8568(1)nm,β=92.799(6)°,Z=4,μ=1.084mm^-1,R=0.0440。两个晶体中镍原子由多啮配体的二个酰氧原子和二个肼氮原子形成平面正方形配位。对配合物的红外光谱进行归属。     

Synthesis, Crystal Structure and Cytotoxic Activity of a Novel Nickel(II) Complex with Schiff Base Derived from Salicylhydrazide

A novel Schiff base complex with π-conjugated system, [Ni(L1)2(py)2] 1 (L1 = (E)-N'-(2,4-dichlorobenzylidene)-2-oxidobenzohydraizide), was synthesized and characterized by elemental analysis and single-crystal X-ray determination. Complex 1 crystallizes in the monoclinic system, space group P21/n with a = 12.8286(10), b = 16.3573(13), c = 19.0206(14) , β = 108.2920(10)o, V = 3789.6(5) 3, Z = 4, Mr = 833.17, Dc = 1.460 g/cm3, μ = 0.843 mm-1, F(000) = 1704, the final R = 0.0537 and wR = 0.0640 for 3836 observed reflections with I > 2σ(I). In the molecular structure of 1, the NiII atoms are six-coordinated by two N and two O atoms from two Schiff base ligands (L1) and two N atoms from two pyridine solvent molecules to form a distorted octahedral geometry. The cytotoxic activities of complex 1 have been experimentally studied against a human HeLa cell in vitro.     

含双二苯基膦乙烷镍配合物的合成与性质

在氯访中通过取代反应制备了含双二苯基膦乙烷（ｄｐｐｅ）的镍配合物［Ｎｉ（ｄｐｐｅ）Ｃｌ_２］,并通过元素分析、热分析、红外光谱、核磁、电导测定、光电子能谱及Ｘ－射线单晶分析表征了配合物的结构和性质,晶体属于单斜品系,空间群为ｐ２_１／ｃ。晶胞参数如下：ａ＝１１．４２９（２）,ｂ＝１３．３４６（２）,ｃ二１５．９５３（７）Ａ;β＝９９．１３（３）°,Ｖ＝２４０２．５Ａ~３, Ｚ＝４, Ｆ（０００）＝１０８８, Ｄ_（ｃａｌｃ）＝１４６０９· ｃｍ~（－３）, ｐ＝１１．７８２ｃｍ~（－１）, Ｒ＝０．０４４７０, Ｒｗ＝０．０５３５２。分析结果表明,配合物中双二苯基膦乙烷属双齿配体,氯离子是单齿配体．     

Synthesis and Structural Characterization of a Novel Heterodinuclear Vanadium(IV)‐Nickel(II) Complex

A novel V^IV‐Ni^II heterodinuclear complex [VO(cat)₂][Ni(1, 2‐PDA)₂H₂O] ( 1 ) (cat = catechol; 1, 2‐PDA = 1, 2‐propane diamine) was synthesized at low temperature (10 °C) and characterized by IR spectroscopy and X‐ray diffraction. A novel Ni–O=V structure exists in the complex, the vanadyl–catechol moiety and the nickel–diamine moiety are connected by an oxygen bridge; all molecules are further assembled into crystallites by O–H ··· O hydrogen bonds.     

Synthesis,Structure and Magnetic Properties of a Novel Nickel(II) Radical Heterospin Complex with Salicylaldoxime

A novel heterospin complex containing both Ni^II and nitroxide radical ligands: [Ni(salox)₂(NIT4Py)₂] ( 1 ) (salox = salicylaldoxime, NIT4Py = 2‐(4′‐pyridyl)‐4,4,5,5‐ tetramethyl‐imidazoline‐1‐oxyl‐3‐oxide) has been synthesized and structurally characterized. The structure consists of neutral Ni(salox)₂(NIT4Py)₂ moieties bridged by intermolecular hydrogen bonds, forming a one‐dimensional chain structure. Magnetic measurements show intramolecular antiferromagnetic interactions between NIT4Py and Ni²⁺ ion.     

镍(Ⅱ)基双氮杂环卡宾配合物的合成及其晶体结构

以咪唑和取代氯化苄为原料,经氮烷基化反应合成三个氮杂环卡宾(NHC)配体[L1:N,N-二苄基咪唑-2-亚基,L2:N,N-二(4-甲基苄基)咪唑-2-亚基,L3:N,N-二(4-氯苄基)咪唑-2-亚基];再以咪唑官能团化的N-杂环卡宾配体和氯化镍为原料,通过金属交换反应合成三个新型的镍基双氮杂环卡宾配合物[Ni(NHC)_2]Cl_2(C1~C3),其结构经~1H NMR,IR,元素分析和X-单晶射线衍射表征。配合物C1和C3属于单斜晶系,分别为P2_1/n和P2_1/c空间群。配合物C2属于三斜晶系,为P1空间群。C1~C3的CCDC分别为:1433176,1433177和1433179。     

牛磺酸缩5-溴水杨醛席夫碱合镍(II)配合物的合成及晶体结构

The reaction of Ni(Ac)₂, Taurine, 5-bromo-salicylaldehyde afford a complex, [Ni(C₉H₈BrNO₄S)(H₂O)₃]·H₂O. Its structure has been determined by single crystal X-ray diffraction. It crystallizes in monoclinic, P2₁/c, a=1.479 98(6) nm, b=1.397 97(6) nm, c=0.746 60(3) nm, β=99.364(2)°, V=1.524 11(11) nm³. Nickel(II) coordinated with six atoms, forming a octahedron. These octahedrons are further interlinked by the hydrogen bonds. CCDC: 639681.     

Synthesis, Crystal Structure and Properties of a Novel Tetranuclear Nickel（II） Complex with Azo-enolic-2-hydroxybenzamide

A novel tetranuclear nickel(Ⅱ) complex [Ni4L2(DMF)2(H2O)2·2DMF] (1,H4L=azo-enolic-2-hydroxybenzamide, DMF=N,N-dimethyl-formamide) has been synthesized and characterized by elemental analysis, UV, IR and X-ray single-crystal diffraction characterization. Complex 1 crystallizes in the monoclinic system, space group P21/n with a=8.8944(11), b=14.4583(18), c=18.097(2) , β=90.00(2)o, Z=2 , V=2327.2(5)3 , C40H48N12Ni4O14 , Mr=1155.66, Dc=1.649g/cm 3 , μ=1.672 mm-1 , F(000)=1192, R=0.0392 and wR=0.0958. The local coordination environment around the nickel ions exist a distorted octahedral and quadrangle geometry in the molecular structure. Complex 1 exhibits strong photoluminescent emission in the ultraviolet region at room temperature. The electrochemical studies reveal that redox of Ni 3+ /Ni 2+ in the complex is a quasi-reversible process.     

Synthesis, Crystal Structure and Antimicrobial Activity of a Novel Ni(II) Complex

A new nickel(II) complex, C34H38N8NiO4, has been prepared and charac- terized by X-ray diffraction analysis. It crystallizes in the monoclinic system, space group P21/c with a = 11.715(5), b = 12.328(5), c =11.113(5) , β = 92.589(5)°, Z = 2, Dc = 1.411 g/cm3, μ = 0.658 mm-1, the final R = 0.0427 and wR = 0.1099 for 2229 observed reflections with I > 2σ(I). The complex is a centrosymmetric plane in which nickel(II) is coordinated in a regular octahedron to the ligand phenytoin through the nitrogen atoms of ethylenediamine, imine and amine. The complex was valued for its antimicrobial activity against bacterial strands using the agar diffusion method, and found to be active against the four test bacterial organisms. Preliminary screening for antimicrobial activities showed that the title complex is quite active against standard strains of Salmonella species, Staphylococcus aureus, Bacillus pumilus and Eschierichia coli.     

Molecular and Supramolecular Structures of a Nickel（Ⅱ） Complex with a Macrocyclic Ligand

1 INTRODUCTION The knowledge of all non-covalent interactions, such as strong and weak hydrogen bonds and p…p interactions, is important to the supramolecular chemistry, biochemistry, crystal engineering and material science[1～7]. Several mononuclear complexes of macrocyclic oxamido Schiff base ligands with phenyls have been used as 揷omplex ligands?to design polynuclear complexes[8～11]. Herein we report the molecular and crystal structures, CH贩稯 hy- drogen bonding and p…p stacki…     

Synthesis and Crystal Structure of a Novel Tetranuclear Manganese(II) Complex with a Tripodal Peptide Ligand

1 INTRODUCTION Amides play an important role in the evolution ofnature. The amidate participates in the coordinationof iron with the ligands containing biomolecules, suchas antitumor drug bleomycin[1] and nitrile hydra-tase[2]. Bleomycin is a clinically useful antitumoragent which catalyzes the cleavage of oxidative DNAand oxidizes a number of organic substrates with di-oxygen or H2O2 . This has raised more interest in [3]the coordination of amide complexes[4, . …     

Synthesis, Crystal Structure and Thermal Stability of (Diacetylacetone)(diimidazole)Nickel(II) Complex

1 INTRODUCTION Acetylacetone is well known as the intermediate product of organic synthesis reaction, which can be used as annexing agent in gasoline, lubricant and desiccant in paint. Also it has been found to possess fungicidal and insecticidal activi…     

Synthesis and Crystal Structure of a Novel Polymeric Thiocyanato-Bridged Heteronuclear Complex of Copper(II) and Cadmium(II)

The title polymeric complex of Cu(II) and Cd(II) bridged by thiocyanate, Cu(en)₂[Cd(SCN)₃]₂, has been prepared and its structure determined by X-ray diffraction (XRD) methods. The crystal structure reveals that the Cu(II) atom is in an elongated octahedral coordination formed by two SCN^– anions and two en molecules. The Cd(II) atom is in a distorted octahedral coordination formed by six bridging SCN^– anions. Two different bridging thiocyanate anions exist in the complex. Both 1,1--SCN^– and 1,3--SCN^– anion act a role of bridge ligand and link Cu(II), Cd(II) atoms, and adjacent Cd(II). Cd(II) atoms form the three-dimensional (3-D) network polymeric structure. The IR and UV-Vis spectra have also been investigated.     

Synthesis,Crystal Structure and Nonlinear Optical Properties of Nickel（Ⅱ） Complex with Schiff—base Ligand

1 INTRODUCTION Recently, the transition metal complexes and inorganic clusters have also been investigated as promising nonlinear optical materials[1～3]. In our past work, much more efforts have been made to find potential nonlinear optical derived from thiosemicarbazone and dithio-carbazates[4]. As a continuous study on new nonlinear optical materials among the -electron delocalized systems con- taining mixed sulfur and nitrogen donors[5, 6], we report herein the crystal structure and…     

Synthesis and Crystal Structure of a Novel Cobalt（Ⅱ） Coordination Polymer with 1,2,4,5-Benzenetetracarboxylate

A novel cobalt（II） coordination polymer,[Co（BTEC）1/2]n 1,has been synthesized with Co（NO3）2·6H2O and 1,2,4,5-benzenetetracarboxylic acid （H4BTEC） by the hydrothermal method,and characterized by elemental analysis,IR and single-crystal X-ray diffraction. Crystallographic data for 1： C5HO4Co,Mr = 183.99,monoclinic,space group C2/c,a = 16.619（6）,b = 7.416（3）,c = 8.040（3）A,β = 90.612（4）°,V = 990.8（6） A^3,Z = 8,Dc = 2.467 g/cm^3,μ = 3.390 mm^-1,F（000） = 720,R = 0.0307 and wR = 0.0847 for 912 observed reflections （I 〉 2σ（I））. X-ray crystal structural analysis revealed that each Co（II） adopts a tetrahedral coordination mode to link four separate BTEC ligands via uniform monodentate carboxylate groups and each BTEC ligand possesses an 8-connected geometry to connect eight Co（II） ions. Complex 1 exhibits a rare （4,8）-connected net with （45.6）2（410.614.84） topology.     

Synthesis and Crystal Structure of a New Ternary Complex of Nickel(II) with L-Aspartic Acid and 1,10-Phenanthroline

1 INTRODUCTION Amino acid is the fundamental structure unit ofbiomacromolecules, such as protein and enzyme, andit is also the important biomicromolecular ligandinside the life body. Study on the metal-amino acidcomplex is the basis of understanding …     

Synthesis and Crystal Structure of a New Nickel(II) Complex with Unsymmetric Quadridentate Schiff Base Containing Oxime

1 INTRODUCTION The interest in the complexes of transition met-als with ketoxime ligands[1, 2] as potential modelsfor metal binding sites in ferroverdin[3, 4] hasprompted the investigations on the structures andthe overall coordination geometry of the metalcenters in these complexes. Oxime derivatives areinteresting ligands since the ketoximes are foundto chelate transition metals through the N (oxime)and O (ketone) donors[5～10]. Herein we report thesynthesis…     

Synthesis and Crystal Structure of a Copper(II) Complex with Benzilic Acid and 1,10-Phenanthroline

A new complex [Cu(phen)3][(C6H5)2C(OH)COO]2·6H2O was prepared by self-assembly of benzilic acid, 1,10-phenanthroline (phen), and copper perchlorate. It crystallizes in triclinic, space group P1, with a = 1.14661(17), b = 1.6455(2), c = 1.6457(2) nm, α = 74.779(2), β = 74.904(3), γ = 84.424(3)o, V = 2.8914(7) nm3, Dc = 1.340 g/cm3, Z = 2, F(000) = 1218, GOOF = 1.018, the final R = 0.0643 and wR = 0.1633. The crystal structure shows that the copper ion is coordinated with six nitrogen atoms from six 1,10-phenanthroline molecules, forming a distorted octahedral coordination geometry.     

新型镍配合物的溶剂热合成及其晶体结构

以2-乙氧基-6-亚氨甲基苯酚(HL)为配体,与氨水和Ni(ClO4)2.6H2O经溶剂热法合成了新型镍配合物[Ni(L)2](1),其结构经IR,元素分析和XRD表征。1属三斜晶系,Pī空间群,晶胞参数a=0.843 3(3)nm,b=1.009 4(2)nm,c=1.188 4(2)nm,α=111.16(3)°,β=97.43(3)°,γ=102.43(3)°,V=0.897 2(11)nm3,Mr=387.05,Z=2,Dc=1 433 g.cm-3,F(000)=404,μ=1.105 mm-1,S=1.015。1中Ni2-分别与两个L-上的两个N原子和两个O原子配位,形成了平面四边形几何构型。分子通过一对N-H┈O氢键形成二聚体;二聚体进一步通过N-H┈O氢键和C-H┈Ni氢键的相互作用形成二维网状结构。