Structure and Magnetic Property of a Cobalt(II) Complex Synthesized Through in situ Hydrothermal Reaction

A new cobalt(II) coordination polymer [Co(L₁)(bpy)(H₂O)] · H₂O ( 1 , H₂L₁ = 2‐sulfobenzoic acid and bpy = 4,4’‐bipyridine) was synthesized by in situ hydrothermal reaction. The single‐crystal X‐ray diffraction analysis shows that compound 1 belongs to monoclinic system with space group C2/c. The structure of compound 1 exhibits a 2D framework linked by ligand L₁ and 4,4’‐bpy, of which L1 was produced by in situ hydrothermal reaction of 2‐(pyridinyl‐4‐methylsulfanyl) benzoic acid. The 2D structure was future connected into a 3D framework through hydrogen bonds. The magnetic analysis indicates the presence of weakly antiferromagnetic interaction between adjacent Co²⁺.     

Synthesis, Crystal Structure and Magnetic Properties of Cobalt(II) Complex Involving Imino Nitroxide Radicals

1 INTRODUCTION The synthesis and study of transition metal com-plexes incorporating organic free radicals have arou-sed great interest in the field of molecular magne-tism[1]. Nitronyl nitroxide radicals (NITR), stable or-ganic radicals, have been widely used as molecularunits in the design and construction of magnetic ma-terials[2～5]. These radicals are especially attractivedue to that their donor atoms can assemble an exten-ded coordination geometry with changing magneticcoupling. A…     

Synthesis and Crystal Structures of Nickel(II) and Copper(II) Complexes of Meso-3,6,6,9-Tetramethyl-4,8-Diazaundecane-2,10-Dione Dioxime

The nickel(II) and copper(II) complexes of meso-3,6,6,9-tetramethyl-4,8-diazaundecane-2,10-dione dioxime (meso-HM-PAO) have an intramolecular hydrogen bond between cis oxime groups. [Cu(meso-HM-PAO-H)(H₂O)](NCS) crystallizes in space group P2₁/n with a = 7.692(1), b = 12.028(2), c=20.235(3) Å, β=93.03(1)°, Z = 4 and Dc=1.46 g/cm³. The final R value for this complex was 0.034 for 2223 observed reflections with I ≥ 2.5σ (I). The Cu(II) coordination is a distorted square pyramid. The Cu(II) ion is five-coorinated with the diazadioxime N atoms equatorial and water O atom axial. The Cu(II) is 0.12 Å from the equatorial plane towards the hydrate. The equatorial Cu-N distances span a narrow range, 1.953(3)-1.999(3) Å. The axial Cu-O distance is 2.314(3) Å. The thiocyanate group is almost linear. The intramolecular O ?O hydrogen bond length is 2.479(4) Å. [Ni(meso-HM-PAO-H)](ClO₄) crystallizes in space group P2₁/c with a = 14.774(3), b = 12.752(3), c = 20.035(4) Å, β = 92.94(3)°, Z = 8 and Dc = 1.51 g/cm³. The final R value for the complex was 0.053 for 4794 observed reflections with F ≥ 4σ (F). The coordination about Ni(II) is a slightly distorted square plane. The Ni(II) ion is 0.0673(7) Å from the best plane of the four donor nitrogen atoms away from the perchlorate ion. The Ni-N distances span a narrow range 1.863(4)-1.927(4) Å. There are two molecules per asymmetrical unit resulting in eight molecules being packed in an unit cell; they are bound together by van der Waals interactions. The O-H ?O bonds of these complexes give characteristic infrared absorptions as well as chemical shift of the ¹H NMR signal (Ni complex).     

Synthesis,Crystal Structure and Characterization of Polynuclear Potassium(I), Copper(II) and Cobalt(II) Complex with Acetylacetonethylenediamine

The title complex [K{Cu(acen)}₃]₂[Co(NCS)₄]·1/4CH₃OH (acen = acetylacetonethylenediamine anion) has been prepared and characterized. Single-crystal x-ray analysis reveals that the complex crystallizes in space group P I with a = 11.442(2), b = 15.098(3), c = 28.500(4) Å, α = 82.77(1), β = 83.58(1), γ = 85.07(1)°. The crystal consists of the complex [K{Cu(acen)}₃]⁺ cations, [Co(NCS)₄]^2? anions and methanol molecules. Three [Cu(acen)] molecules function as bridging ligands through phenolic O atoms to one K⁺ to give the tetranuclear [K{Cu(acen)}₃]⁺ cation. Each copper(II) atom in the cation is in a square-planar geometry, being coordinated by two oxygen atoms and two nitrogen atoms from a quadridentate acen ligand. The cobalt(II) atom is coordinated by four nitrogen atoms of thiocyanate ligands, forming a deformed tetrahedral environment. The IR and UV-Vis spectra have also been investigated.     

1,3-Bis(2-alkyltetrazol-5-yl)triazenes and their Fe(II), Co(II) and Ni(II) complexes: Synthesis,spectroscopy, and thermal properties. Crystal structure of Fe(II) and Co(II) 1,3-bis(2-methyltetrazol-5-yl)triazenide complexes

Complexes ML¹₂ and ML²₂, with M = Fe^II, Co^II, Ni^II, and 1,3-bis(2-R-tetrazol-5-yl)triazenide ligands L¹ (R = Me) and L² (R = ^tBu), have been synthesized by the reaction of corresponding 1,3-bis(2-R-tetrazol-5-yl)triazenes with metal(II) salts in basic media and characterized by IR, UV–Vis spectroscopy, thermal and X-ray diffraction analyses. Both 1,3-bis(2-R-tetrazol-5-yl)triazenes were found to deprotonate on coordination and act as tridentate chelating ligands forming distorted MN₆ octahedra around metal(II) cations.     

A New Pt(II) Complex with Anionic s-Triazine Based NNO-Donor Ligand: Synthesis,X-ray Structure,Hirshfeld Analysis and DFT Studies

The reaction of PtCl₂ with s-triazine-type ligand (HTriaz) (1:1) in acetone under heating afforded a new [Pt(Triaz)Cl] complex. Single-crystal X-ray diffraction analysis showed that the ligand (HTriaz) is an NNO tridentate chelate via two N-atoms from the s-triazine and hydrazone moieties and one oxygen from the deprotonated phenolic OH. The coordination environment of the Pt(II) is completed by one Cl⁻¹ ion trans to the Pt-N_(hydrazone). Hirshfeld surface analysis showed that the most dominant interactions are the H···H, H···C and O···H intermolecular contacts. These interactions contributed by 60.9, 11.2 and 8.3% from the whole fingerprint area, respectively. Other minor contributions from the Cl···H, C···N, N···H and C···C contacts were also detected. Among these interactions, the most significant contacts are the O···H, H···C and H···H interactions. The amounts of the electron transfer from the ligand groups to Pt(II) metal center were predicted using NBO calculations. Additionally, the electronic spectra were assigned based on the TD-DFT calculations.     

Synthesis,Spectra, Thermal Analysis and Crystal Structure of Trans-Bis(2-Pyridinepropanol)Bis (Saccharinato)Cobalt(II)

The title complex, [Co(pypr)₂(sac)₂] (pypr = 2-pyridinepropanol and sac = saccharinate), has been prepared and characterized by elemental analysis, electronic and FTIR spectra, magnetic susceptibility measurements, thermal analysis and X-ray diffractometry. The complex crystallizes in triclinic space group PI with a = 8.1836(2), b = 10.0062(2), c = 10.4989(3) Å, α = 90.474(1), β = 107.989(1) and γ = 110.923(1)°. The cobalt(II) ion sits on a center of symmetry and is octahedrally coordinated by two pypr and two sac ligands. Both pypr and sac ligands occupy the trans positions of the coordination octahedron. The two pypr ligands are neutral and act as bidentate N- and O-donor ligands forming two symmetry-related seven-membered chelate rings around the cobalt(II) ion, while both sac ligands are O-coordinated through the carbonyl oxygen atoms. On heating the endothermic removal of two pypr ligands occurs in the first stages of decomposition and at higher temperatures the Co/sac intermediate decomposes to Co₃O₄ and finally to CoO.     

一维链状镉配合物的合成及结构表征

在甲醇体系中合成了镉配合物[Cd(L)₂(H₂O)₂](ClO₄)₂·MeOH (1)[L=1,3,5-三(3-吡啶基甲氧基)苯]。通过元素分析及X-射线单晶衍射对其进行了表征。结构分析结果表明该化合物属于三斜晶系,P1空间群,晶胞参数为a=1.057 1(5) nm,b=1.059 0(5) nm,c=1.270 8(7) nm,α=87.460(16)°,β=81.895(17)°,γ=62.326(14)°,晶胞体积V=1.247 0(11) nm³,Z=1,D_calc=1.569 g·cm^-3,F(000)=604,μ=6.26 cm^-1,R=0.035 2,wR=0.066 4。在化合物1中,每个Cd(II)的配位环境为变形八面体,而每个配体L通过其两个吡啶基团连接2个Cd(II)形成一维链状结构,并进一步通过O-H…N,O-H…O和C-H…O氢键作用形成了一个具有三维结构的超分子化合物。     

Synthesis and Crystal Structure of Copper(II) Complex with N-Acetoxyl-picolinamide

1 INTRODUCTION The picoloylhydrazide compounds are close to thebiologic environment and can react with microele-ments in organism so as to have antitubercular andantineoplastic activities. However, owing to the exis-tence of amino group, this kind of compounds aretoxic to some extent[1]. In order to decrease theirtoxicity, hydrazone or hydrazide compounds synthe-sized by the condensation reaction of amino and car-bonyl groups have been well studied in recentyears[1～7]. Herein we report t…     

Synthesis, Crystal Structure and Magnetic Properties of a New Zn(II)-Nitronyl Nitroxide Complex

A new complex [Zn(NIT-1'-MeBzIm)Cl2(H2O)] (NIT-1'-MeBzIm = 2-{2'-[(l'- methyl)benzimidazolyl]}-4,4,5,5-tetramethylimidazoline-1-oxyl-3-oxide) has been prepared and structurally characterized by X-ray diffraction method. Crystal data: monoclinic, space group P21/n, Z = 4, C15H21Cl2N4O3Zn, Mr = 441.63, a = 7.2225(10), b = 30.849(4), c = 8.8758(13) , β = 103.904(2)°, V = 1919.6(5) 3, Dc = 1.528 g/cm3, μ(MoKα) = 1.579 mm1, F(000) = 908, R = 0.0436 and wR = 0.1029 for 2456 observed reflections with I > 2σ(I). X-ray analysis reveals that the Zn(II) ion is four-coordinated with a distorted tetrahedron. There also exist H-bonds, π-π piling interactions and weak intermolecular contacts between the NO groups which form a mutual stagger 3-D network configuration. Magnetic investigation reveals that there exists intermolecular antiferro- and ferromagnetic interactions in the title complex.     

Synthesis,Crystal Structure and Magnetic Property of Copper(II) Complex with 4′-Cyanobenzyl-1-imidazol

A neutral mononuclear complex [Cu(cbIm)₄(NO₃)₂] (cbIm = 4'-cyanobenzyl-1-imidazol) was synthesized and characterized by x-ray crystallography. It crystallizes in the triclinic space group P-1 with a = 8.249(2), b = 8.735(2), c = 16.597(2) Å, f = 81.980(10), g = 88.540(10), n = 63.570(10)° and Z = 2. The final refinement of the structure leads to R and Rw of 0.0394 and 0.0991, respectively. The crystal structure of the complex indicates a distorted octahedral environment around the Cu(II) atom, coordinated by four imidazole N atoms of four cbIm and two O atoms of two nitrates. Magnetic measurements show that the complex exhibits Curie behavior.     

Synthesis,Crystal Structure and Magnetic Properties of a Terephthalato-bridged Binuclear Nickel(II) Complex

A new terephthalato-bridged binuclear nickel(II) complex with a tetraazamacrocyclic compound as the terminal ligand, [Ni 2 (cth) 2 (µ-TPHA)](ClO 4 ) 2 (1) [cth= rac -5,7,7,12,14,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane] has been synthesized and characterized. According to X-ray crystallographic studies on the solvated species 1·2CH 3 OH, each Ni(II) ion lies in a distorted octahedral environment, and the terephthalato ligand bridges two Ni(II) ions in a bis bidentate fashion. Cryomagnetic measurements revealed Curie-Weiss behaviour with è = m 1.4 K. Such behaviour may be due to a very weak intramolecular superexchange interaction through the extended bridge, a weak intermolecular exchange interaction or the local zero-field splitting of Ni(II) ions.     

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.     

Synthesis and Crystal Structure of Dichlorobis(1-methylimidazoline-2(3H)-thione-S) Cobalt(II)

The reaction of anhydrous cobalt(II) dichloride with 1-methylimidazoline-2(3H)thione in dichloromethane solution gave the title complex, [Co(C4H6N2S)2Cl2]. X-ray single-crystal analysis revealed that the complex crystallizes in a monoclinic system, space group P21/c, a = 13.9707(10), b = 10.0435(7), c = 10.3910(6) (A), β = 91.181(3)o, V = 1457.70(17) (A)3, Z = 4, C8H12Cl2N4S2Co, Mr = 358.17, Dc = 1.632 g/cm3, μ = 1.813 mm-1, F(000) = 724, the final R = 0.0710 and wR = 0.1224 for 1549 observed reflections with I > 2((I). The Co atom is coordinated by two S atoms from two 1-methylimidazoline-2(3H)-thione ligands and two chloride ions in a slightly distorted tetrahedral geometry. The intramolecular classical hydrogen-bonding interactions involving chloride ions and N-H groups of the heterocyclic thione ligands are observed. The offset π-π stacking interactions between the imidazole rings of adjacent molecules with a face-to-face distance of 3.604 (A) are found in the packing diagram.     

Synthesis,Crystal Structure and Magnetic Properties of an Oxalato-Bridged Dinickel(II) Complex Containing A MacrocyClic Ligand

A new binuclear nickel(II) complex [Ni(µ-C₂O₄)(rac-cth)₂](ClO₄)₂[rac-cth = rac -5,7,7,12,14,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane] has been prepared and its structure determined. It consists of centrosymmetric [Ni( µ -C₂O₄)(rac-cth)₂]²⁺ cations separated by perchlorate anions, with a centre of symmetry lying in the middle of the C-C bond of the bis-bidentate oxalate bridge. The tetraazamacrocycle adopts a folded conformation around the nickel atom, which is six coordinated in a distorted octahedral arrangement. Variable temperature magnetic susceptibility measurements (4-300 K) suggest a moderate intramolecular antiferromagnetic interaction between the metal ions ( J = -34.0 cm^-1, g = 2.07)     

烷氧桥联混合配位的双核铜配合物的合成、结构及量子化学计算

0IntroductionThere has been intensive interests in the past fewyears for planar Cu-(μ-OR)-Cu dinuclear systems inwhichμ-OR=OH-,MeO-,EtO-[1￣5],especially for themagnetic behavior of planar[N2Cu(μ-OH)]systemsand the magneto-structural correlation between theangle Cu-O-Cu and the magnetical exchange parame-ter J[6,7].Some hydroxo-bridged Cu!compounds alsohave catalytic activity[8].In addition,low-molecular-weight Cu!coordination compounds with nitrogen-containing donors have frequent…     

1,3-双(2-苯并咪唑基)-2-氧杂丙烷与锌配合物的合成、晶体结构及其与DNA作用方式的研究

合成了1,3-双(2-苯并咪唑基)-2-氧杂丙烷合锌(II)配合物, 并用元素分析和X射线衍射进行了表征, 表明其为畸变八面体构型. 用紫外、DNA熔点、荧光、粘度等手段对其与小牛胸腺DNA作用方式进行了研究. 实验结果表明, 由于配合物的八面体构型以及苯并咪唑环的平面性, 其与DNA作用方式可能为部分插入.     

Crystal structure and chemical bonding in tin(II) acetate

Tin(II) acetate was prepared and its crystal structure was solved from X-ray powder diffraction data. Tin(II) acetate adopts a polymeric structure consisting of infinite Sn(CH₃COO)₂ chains running along the c-axis which are packed into groups of four. The acetate groups bridge the Sn atoms along the chains. The Sn atoms are asymmetrically surrounded by four oxygen atoms with two short Sn–O distances (2.170(6), 2.207(6) Å) and two longer ones (2.293(7), 2.372(8) Å). The coordination environment of the Sn atoms is completed up to a strongly distorted trigonal bipyramid SnO₄E by the sterically active lone electron pair E. The coordination environment of the Sn atoms is virtually identical for Sn(CH₃COO)₂ in the gaseous and solid phase: the two short Sn–O bonds and the lone electron pair are located in the equatorial plane of the trigonal bipyramid and the two longer Sn–O bonds are directed towards the apical vertexes. Localization of the lone electron pair on Sn(II) was confirmed by electron localization function (ELF) analysis. The polymeric nature of the tin(II) acetate crystal structure was confirmed by a MALDI-TOF experiment.     

Crystal Structure and Magnetic Properties of a Copper(II) Chloride Complex with Nitronyl Nitroxide

A new compound [Cu(NITPhCH₃)₂Cl₂] (NITPhCH₃ 2-(4-methyl-phenyl)-4,4,5,5-tetramethyl-imidazoline-1-oxyl-3-oxide) has been characterized spectroscopically. A crystal structure analysis has shown the copper ion to be planar, coordinated by two chlorine atoms and two oxygen (nitroxyl) atoms. Based on magnetic susceptibility measurements the compound was found to exhibit a moderately strong antiferromagnetic interaction (J= m 107.44 cm_-1) between copper(II) and the radical.     

A Fluorescent Cobalt（II） Complex for the Recognition of Cations and Small Molecules： Synthesis, Structure and Characterization

A fluorescent cobalt(Ⅱ) complex, 1 [Co(H2bibim)2(5-nipa)], for the recognition of cations and small molecules constructed with 5-nitroisophthalic acid (5-H2nipa) and 2,2-biben-zimidazole(H2bibim) has been synthesized by hydrothermal methods and structurally characterized by elemental analysis, IR spectroscopy, PL and single-crystal X-ray diffraction. The cobalt units are six-coordinated by two H2bibim ligands and one 5-nitroisophthalic acid group, which are further connected into a three-dimensional (3D) network by intermolecular hydrogen bonds. Complex 1 exhibits fluorescence and thus has detection capabilities for different cations and small solvent molecules in the solution state at room temperature.